最新刊期

    44 5 2025

      Special Topic

    • WAN Yuan-yuan, LIU Chun, LIU Zhi-min, XU Zhi-gang
      Vol. 44, Issue 5, Pages: 759-773(2025) DOI: 10.12452/j.fxcsxb.25021386
      Research Progress of Molecular Imprinting Technology and Its Application in the Detection of Bisphenols
      摘要:Bisphenol environmental estrogens are well-known endocrine disruptors. As a branch of emerging pollutants,they have attracted the attention of many countries in the world due to their environmental persistence,bioaccumulation,biotoxicity and refractory degradation in the environment. Therefore,highly sensitive detection of bisphenol environmental estrogens in environmental,food and biological samples is essential. Traditional sorbents have disadvantages,such as long time consuming,large amount of use,and poor enrichment effect of trace pollutants,which affect the accuracy of quantification. Therefore,there is an urgent need to develop and design new materials with high selectivity and enrichment properties as adsorbents for pretreatment technologies to achieve highly selective and sensitive analysis of environmental estrogens in bisphenols. Molecular imprinting has been widely used for the enrichment of trace pollutants due to its structural predictability,recognition specificity and application universality. This review introduces the principle and recognition mechanism of molecular imprinting technology,and focuses on recent synthesis strategies of molecular blots and their application as sample pretreatment sorbents in the analysis of bisphenol environmental estrogens in environmental,food and biological samples. Furthermore,it summarizes the problems of molecular imprinting technology in the detection of bisphenol type environmental estrogens and looks forward to its development trend.  
      关键词:molecular imprinting technique;bisphenol;environmental estrogens;emerging pollutants;sample pretreatment   
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      Scientific Papers

    • YOU Qian, Manabu Fujii, FU Qing-long
      Vol. 44, Issue 5, Pages: 774-780(2025) DOI: 10.12452/j.fxcsxb.240826345
      Chemodiversity of Dissolved Organic Matter in Seawater of Tokyo Bay Affected by Sunlight Irradiation
      摘要:The effect of natural sunlight irradiation on the chemodiversity of coastal seawater dissolved organic matter in the coastal seawater of Tokyo Bay was investigated by Fourier transform-ion cyclotron resonance mass spectrometry(FT-ICR MS). Results of this study revealed that the CHO,CHOS,and CHON compounds with low aromatics were dominant in the coastal seawater dissolved organic matter(DOM) of Tokyo Bay,Japan. After natural sunlight irradiation,the number of tannins-like and N-free saturated compounds increased by 60% and 62%,respectively. In addition,the intensity of the normalized ion peaks(the intensity of the ion peak was normalized by the concentration of organic carbon) of 2 347 lignin-like and 616 saturated compounds decreased by the natural sunlit irradiation;while the intensity of normalized ion peaks of 2 211 lignin-like,975 saturated compounds,493 tannins-like,and 289 aminosugars increased by the natural sunlight irradiation. The results of this study will deepen the understanding of chemodiversity in coastal seawater DOM and provide valuable insights for the photochemical and environmental effects of aquatic DOM.  
      关键词:coastal seawater;dissolved organic matter;ultrahigh-resolution mass spectrometry;sunlight-irradiated;molecular composition   
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    • LI Chang-sheng, GAO Shu-hui
      Vol. 44, Issue 5, Pages: 781-793(2025) DOI: 10.12452/j.fxcsxb.240925415
      Determining the Sequence of Intersecting Lines Based on Vis-NIR Hyperspectral Imaging Technology
      摘要:In the field of forensic questioned document examination,the analysis of the ink of the text and the seal imprint formation time sequence is the key technology to verify the authenticity of the instrument material evidence. This paper proposes a sequence of intersecting lines identification model that combines visible-near infrared hyperspectral imaging(Vis-NIR HSI) and convolutional neural networks(CNN). A dataset of hyperspectral data from 42 000 different red-black ink sequence samples was collected.The samples were preprocessed using median filtering(MF),Savitzky-Golay smoothing(SG smoothing),multiplicative scatter correction(MSC),and normalization methods. Further,the successive projection algorithm(SPA) and competitive adaptive reweighted sampling(CARS) were employed for spectral feature wavelength selection. Several binary classification machine learning models,including logistic regression(LR),and a one-dimensional convolutional neural network(1D-CNN) model were developed and their modeling effects compared. The results showed that the CARS-1D-CNN model,established using feature wavelengths extracted by the CARS method,achieved the best classification performance with accuracies of 96.98% on the training set and 95.54% on the test set. The study demonstrates that the combination of Vis-NIR HSI and 1D-CNN can effectively identify the sequence of intersecting lines. This method,in conjunction with conventional examination techniques,can further enhance the accuracy and efficiency of forensic questioned document examination.  
      关键词:visible-near infrared hyperspectral imaging(Vis-NIR HSI);questioned document examination;sequence of intersecting lines;machine learning;1D-CNN   
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    • CHEN Kui, HUANG Bei-bei, LIU Jie, WANG Teng-teng, QIAO Yun, CAI Sheng-nan, SHI Li-xia, LI Yue-ting, XIAO Hong-bin
      Vol. 44, Issue 5, Pages: 794-803(2025) DOI: 10.12452/j.fxcsxb.241114528
      Study on Identification and Rapid Determination of Multiple Components of Zhutong Granules
      摘要:Forty-nine components of Zhutong granules were identified based on ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF-MS/MS). Using high performance liquid chromatograph multi-wavelength detector(HPLC-MWD),a rapid determination method of 12 important chemical constituents in Zhutong granules was established with the aid of multiple dual wavelength switching. The Agilent Poroshell 120 EC-C18 chromatographic column(4.6 mm × 100 mm,2.7 μm) was used with 0.1% formic acid water-acetonitrile as the mobile phase for gradient elution. The flow rate was set at 1.2 mL·min-1 with column temperature of 30 ℃ and injection volume of 5 μL. Dual AJS ESI ion source quadrupole time-of-flight mass spectrometry was used to collect accurate molecular weight and fragment ion in positive and negative ion modes. Through the establishment of Zhutong granules component database,49 major chemical components were screened and identified by accurate molecular weight matching,fragment ion and reference substance comparison. Dual wavelength switching(0-2 min,17-21 min,23-25 min,220 nm;2-17 min,21-23 min,283 nm) were used to determine 12 main components in Zhutong granules quantitatively within 25 min. Twelve major components reached baseline separation in dual-wavelength switching chromatograms with quantitation limits of 0.050 0-0.655 0 μg·mL-1. and recoveries of 98.3%-103%. The average contents of 12 components in 3 batches of Zhutong granules were 0.060-16.597 mg·g-1. This method can rapidly determine more components with good sensitivity and accuracy,which is useful for quality control and subsequent new drug development of Zhutong granules.  
      关键词:Zhutong granules;chemical identification;multiple component quantitative analysis;dual wavelength switching   
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    • WU Lei, ZHANG Xin-tong, LIU Zi-yan, ZHANG Tian-xing, ZHU Qian-wan, LI Qi-yu, QIE Xue-jiao, DU Shan-shan
      Vol. 44, Issue 5, Pages: 804-810(2025) DOI: 10.12452/j.fxcsxb.240913397
      Identification of Microplastics in Urine by Laser Direct Infrared Spectroscopy
      摘要:Agilent 8700 laser direct infrared spectroscopy was used to investigate microplastics in urine from school-aged children and adults in this study. An analytical method for detecting microplastics in human urine was established,and detailed data on the types,quantities,and particle size distribution of microplastics in two age groups were obtained. The results revealed the detection of 304 particles in the urine of 21 school-aged children,primarily consisting of high-density polyethylene,polyvinyl chloride,polyamide,and polyethylene. In contrast,42 particles were detected in the urine of 6 adults,predominantly comprising polyvinyl chloride,polyamide,polyethylene,and polypropylene. Notably,microplastics with small particle sizes(20-70 μm) constituted a high proportion in both sample groups,accounting for 92.0% and 95.2%,respectively. Comparative analysis indicated the widespread presence of microplastics in urine,with distinct differences in quantity and chemical composition between the two groups,which may be related to the children's behavior habits,respiratory and metabolic characteristics,and living environment. This research furnishes crucial insights into the exposure of microplastics within the human body,aiding in the assessment of microplastic risks faced by individuals across different age groups.  
      关键词:microplastics;laser direct infrared spectroscopy;urine;school-age children;adult   
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    • ZHANG Lei, WANG Si-ya, ZHANG Yun-tao, REN Qiang
      Vol. 44, Issue 5, Pages: 811-821(2025) DOI: 10.12452/j.fxcsxb.240913396
      Determination of 13 Heparan Sulfate Disaccharides in PANC-1 and CFPAC-1 Cells Tumor Bearing Mice with Pancreatic Cancer by Precolumn Derivatization/High Performance Liquid Chromatography and Fluorescence Detection
      摘要:A precolumn derivatization/high performance liquid chromatography-fluorescence detection(HPLC-FLD) method for the determination of 13 heparan sulfate(HS) disaccharides in PANC-1 and CFPAC-1 cells tumor bearing mice with pancreatic cancer was established. HS disaccharides were obtained from pancreatic cancer samples by defatting and protease enzymatic hydrolysis,and then reacted with 2-aminoacridone(AMAC) derived reagents. The separation was performed by Thermo Scientific HYRERSIL ODS-2 C18 column,and the mobile phase gradient elution was performed with methanol-60 mmol/L ammonium acetate(pH 5.6) at excitation wavelength of 425 nm and emission wavelength of 520 nm. The results showed that the 13 HS disaccharides had a good linear relationship within the corresponding mass concentration ranges(r2≥0.999 0),with detection limits(LODs) of 0.012-0.313 µg/mL and the quantitation limits(LOQs) of 0.117-1.250 µg/mL. The relative standard deviations(RSDs) of precision ranged from 0.040% to 0.63%,the RSD of intra-day stability ranged from 0.34% to 3.6%,the RSD of inter-day stability ranged from 1.8% to 6.4%. The recoveries ranged from 80.7%-109%,and RSD was 0.50%-17%. 9 HS disaccharides were detected in the tumor tissue of the two types of pancreatic cancer cells,among which ΔUA-GlcN(ⅣH) accounted for the highest proportion,with concentrations of 28 627.558 nmol/g and 66 938.786 nmol/g,respectively. ΔUA-GlcNAc(ⅣA) and ΔUA-GlcN,6S(ⅡH) took the second place,and the results of molecular docking showed that ⅣH had the strongest binding force with heparin-binding epidermal growth factor(HB-EGF) and ⅡH had the strongest binding force with fibroblast growth factor-2(FGF-2). The characteristics of HS sulfated sequence and its interaction with HB-EGF and FGF-2 regulate the occurrence and development of pancreatic cancer. The findings of this study may provide valuable insights for the early treatment and diagnosis of pancreatic cancer.  
      关键词:pancreatic cancer;heparan sulfate(HS);HPLC-FLD;precolumn derivatization   
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    • GONG Jia-hui, XIANG Jie, ZOU Jian-dong, ZHOU Qing, LI Chang-yin
      Vol. 44, Issue 5, Pages: 822-835(2025) DOI: 10.12452/j.fxcsxb.241030499
      Systematic Screening and Identification of Chemical Constituents in Yan Ling Yi Shou Formula Based on UPLC-Q-TOF-MS/MS Technology
      摘要:Ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS) technology was used to systematically and comprehensively characterize the chemical components of Yan Ling Yi Shou Formula(YLYSF). A Waters ACQUITY UPLC® HSS T3 column(2.1 mm×100 mm,1.8 μm) was used for the separation,with an injection volume of 5 µL and mobile phases of 0.1% formic acid solution and 0.1% formic acid acetonitrile solution in a gradient elution at a flow rate of 250 µL/min. Both positive and negative ion monitoring modes were implemented for the electrospray ionization source(ESI).The identification of compounds was conducted through the MS and MS/MS data,reference standards,database,and literature reports. 113 chemicals in all were examined and determined from YLYSF,including 32 terpenoids,24 flavonoids,16 phenylpropanoids,12 organic acids,4 benzoquinones and 25 other compounds. This study laid the foundation for the chemical substances of YLYSF. The results of this study can serve as a basis for further research on the development of standards for evaluating quality,the selection of active ingredients,and the clarification of the formula’s mechanism of action.  
      关键词:Yan Ling Yi Shou Formula;UPLC-Q-TOF-MS/MS;systematic screening;chemical constituents;fragmentation pattern   
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    • HUANG Yun-jia, LI Wen, DUAN Min-min, WANG Xiao-yun, ZHANG Xiao-ping, CHEN Huan-wen
      Vol. 44, Issue 5, Pages: 836-843(2025) DOI: 10.12452/j.fxcsxb.240831358
      Mass Spectrometry Study on Distinguishing the Position of Hexenol Carbon-Carbon Double Bond Based on Water Radical Cation
      摘要:Different double bond positional isomers of hexenol have different biological activities. Rapid and accurate identification of their carbon-carbon double bond positional isomers helps to better understand their structure and biological functions. In this study,a method based on water radical cations to distinguish the position isomers of the carbon-carbon double bond of hexenol was established. The specific strategy is:first,a large number of water radical cations were prepared by low-energy corona discharge technology,and then the hexenol molecule was introduced to react with the water radical cation to form the epoxidation product m/z[M+O]+•,and then the obtained epoxidation product was subjected to collision induction analysis to form a series of characteristic fragment ions m/z 60,m/z 74,m/z 88,locate the double bond,thereby distinguishing the position of different carbon-carbon double bonds. The advantages of this method include rapid reaction,rapid and accurate mass spectrometry analysis.The experimental device is simple,without reaction pretreatment,and the experiment is simple. In addition,the reaction process does not require additional organic solvents and is environmentally friendly.  
      关键词:carbon-carbon double bond;location heterogeneity;water radical cation;hexenol;mass spectrometry   
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    • WANG Jia-ding, TANG Gao, LU Yan, LU Heng-jun, YE Tao, SHI Rui-rui
      Vol. 44, Issue 5, Pages: 844-852(2025) DOI: 10.12452/j.fxcsxb.240729260
      Determination of 29 Trace Impurity Elements in Electronic-grade Phosphoric Acid Using Triple-quadrupole Inductively Coupled Plasma Mass Spectrometry
      摘要:A method for determining the content of 29 trace impurity elements in electronic-grade phosphoric acid using triple-quadrupole inductively coupled plasma mass spectrometry(ICP-MS) in an ultra-clean environment was established. The use of a Class 100 cleanroom and a dynamic Class 10 sample introduction chamber effectively controlled contamination.By optimizing instrument parameters,the element response intensity was improved,and the oxide conversion rate was reduced to avoid mass spectrometric interference caused by oxide ions. The standard addition method was used to match the matrix effect,and a combination of multiple reaction modes including He mode,O2 mode,and Cool-NH3 mode was employed. This effectively avoided various polyatomic ion interferences generated from Ar plasma and phosphoric acid matrix side reactions,reduced the method detection limits,and improved quantitative accuracy. The results showed that the linear correlation coefficients for the 29 trace elements were all greater than 0.998 in the range of 0-100 ng/kg,the method detection limits in 1%(w/w) phosphoric acid solutions ranged from 0.03 to 3.39 ng/kg,the spiked recoveries were 77.6% to 112%,and the stability RSD was not more than 7.0%. These results are reliable and meet the requirements for determining electronic-grade phosphoric acid used in advanced processes.  
      关键词:triple-quadrupole inductively coupled plasma mass spectrometry (ICP-MS/MS);electronic-grade phosphoric acid;trace elements;advanced production process   
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    • HU Shuang, WU Lei, HUANG Yu, YAO Xiao-fei, HUA Zhen-dong
      Vol. 44, Issue 5, Pages: 853-859(2025) DOI: 10.12452/j.fxcsxb.241023476
      Rapid Separation and Detection of Phenethylamines Isomers by Ultra Performance Convergence Chromatography-Mass Spectrometry
      摘要:Phenethylamines are widely abused currently as a class of new psychoactive substances(NPS). They are characterized by a wide variety of types,high potential harm and the presence of a large number of isomers. The structure and properties of these isomers are very similar,and thus pose great challenges for their accurately distinguishment and identification. In this study,an ultra performance convergence chromatography-mass spectrometry method for the rapid separation and detection of phenethylamines positional isomers and carbon chain isomers was established by using a Waters ACQUITY UPC2 BEH column,supercritical fluid CO2 as primary mobile phase,20 mmol/L ammonium formate in methanol as modifier and the column temperature at 60 ℃. Basic or baseline separation of 12 isomers could be achieved within 8.0 minutes. The limit of detection was between 0.02-0.5 ng/mL and the relative standard deviations of retention time were less than 0.30%. Compared with conventional ultra-high performance liquid chromatography-mass spectrometry method,this method is much better in the separation efficiency of isomers,which provides a new means for the accurate qualitative analysis of phenethylamines.  
      关键词:ultra performance convergence chromatography;mass spectrometry;phenethylamines;isomers;new psychoactive substances   
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    • LU Duan-ping, CHENG Jia-hua, HONG Qing-ling, CHEN Xu, CHEN Shuo, JIAN Yu-ying, ZHENG Jing-feng, CHEN Zai-min
      Vol. 44, Issue 5, Pages: 860-867(2025) DOI: 10.12452/j.fxcsxb.241015468
      Determination of 16 Benzene Series in Sunscreen Cosmetics by Headspace-Gas Chromatography-Mass Spectrometry
      摘要:In this study,a method for the detection of 16 benzene series in sunscreen cosmetics was established based on headspace-gas chromatography-mass spectrometry(HS-GC-MS). The samples were dispersed with methanol and diluted with water,then equilibrated at 80 ℃ for 40 min.The samples were separated on a HP-5MS capillary column(30 m×0.25 mm×0.25 μm),then detected by GC-MS in selected ion monitoring mode(SIM). Toluene-D8 and 1,2-dichlorobenzene-D4 were used as internal standards and matrix matching curves were used for quantitative analysis. The results showed good linearity(r≥0.997 4) for 16 benzene series in corresponding concentration ranges. The limits of detection were in the range of 0.02-0.06 μg∙g-1. The average recoveries of two substrates at three different spiked levels ranged from 90.0% to 103%,with the relative standard deviations(RSDs) ranged from 0.20% to 6.5%. The method was used to detect 60 batches of sunscreen cosmetics,benzene series were detected in 39 batches of samples,among which the detection rates of m-xylene & p-xylene,o-xylene,toluene and ethylbenzene were 45%,32%,16% and 16%,respectively. Benzene was detected in five batches of sunscreen spray products,with content exceeding the limit(2.0 mg∙kg-1) in the “Safety and Technical Standards for Cosmetics”(2015 edition) . The content of o-xylene,1,3,5-tritylene and m-xylene & p-xylene in some samples exceeded 2.0 mg∙kg-1. The method is simple,rapid,sensitive and accurate,which can be used for the determination of 16 benzene series in sunscreen cosmetics.  
      关键词:headspace-gas chromatography-mass spectrometry;cosmetics;benzene series;content determination   
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    • TANG Yun-xi, BAI Ya-min
      Vol. 44, Issue 5, Pages: 868-875(2025) DOI: 10.12452/j.fxcsxb.240816310
      Determination of 25 Anesthetics in Aquatic Products Using QuEChERS Coupling with Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry
      摘要:This study analyzed 25 anesthetics in aquatic products using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) in combination with QuEChERs pretreatment technology. Samples were extracted with acetonitrile after soaked in water and cleaned up using a sorbent mixture of octadecyl bonded silica gel(C18),N-propylethylenediamine(PSA) and carbon black(Carb). The extracts were chromatographically separated using a Waters HSS T3 columnfollowed by MS detection in multiple reaction monitoring(MRM) mode. Eugenol compounds were determined using acetonitrile and water as mobile phases in positive and negative ESI modes,while caine anesthetics,quinalidine and diazepam were determined with a mobile phase of acetonitrile-0.1% formic acid water in positive ESI mode. Under optimized conditions,good linearity was observed for the 25 anesthetics in the range of 1-50 ng/mL,with specific compounds like 3-aminobenzoic acid,4-aminobenzoic acid,and 6 eugenol compounds demonstrated linearity within the ranges of 10-500 ng/mL. The limits of quantitation(S/N=10) were 1-10 µg/kg. Average recoveries at three spiked levels ranged from 65.2% to 112%,with relative standard deviations(RSDs) of 2.1%-11%(inter-batch,n=6) and 2.3%-11%(intra-batch,n=3). This method is simple,sensitive and specific,making it suitable for the rapid qualitative and quantitative analysis of anesthetics in aquatic products.  
      关键词:QuEChERS;ultra-performance liquid chromatography-tandem mass spectrometry;aquatic products;anesthetics   
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    • WANG Zi-qing, MENG Zi-xuan, HAO Li-ping, ZHANG Ruo-yu, ZHANG Hao-ran, LIU Kai-xuan, KANG Wei-jun, AI Lian-feng
      Vol. 44, Issue 5, Pages: 876-883(2025) DOI: 10.12452/j.fxcsxb.241024481
      Determination of Nine Bile Acids in Dried Blood Spots by Precolumn Derivatization-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry
      摘要:A highly efficient and reliable precolumn derivatization-high performance liquid chromatography-triple quadrupole mass spectrometry method was established for the determination of nine types of bile acids in dried blood spots. Samples were extracted by vortexing with methanol and extracted by vortexing with methanol. After derivatization with a 2-hydrazinopyridine acetonitrile solution,the samples were dried,redissolved in a 50% methanol aqueous solution,filtered through a 0.22 µm organic membrane,and quantitatively analyzed using the internal standard method. The T3 chromatographic column was selected,and a gradient elution was carried out using water(0.1% formic acid)-methanol acetonitrile(9∶1,volume ratio) as the mobile phase. Scanning was performed in the positive ion mode,and detection was carried out in the multiple reaction monitoring mode. The results showed that the standard curves of nine target substances exhibited an excellent linear relationship,with the correlation coefficients ranging from 0.998 2 to 0.999 8. The limits of detection(LODs) were between 0.2 nmol/L and 2.0 nmol/L,and the limits of quantification(LOQs) were between 1.0 nmol/L and 10 nmol/L. The recoveries ranged from 92.4% to 109%,and the relative standard deviations(RSDs) were all less than 15%. Both the intra-batch and inter-batch RSDs were less than 12%. The relative matrix effects were between 89.6% and 109%(RSD≤11%),and the derivatization products could be stored at 4 ℃ for 48 hours. Compared with the results of serum samples,this method showed a high degree of correlation and consistency. This method had good selectivity and linear relationship,with no obvious matrix effect or carryover effect. The target substances exhibited good stability,and the method could be used for the rapid detection of bile acids in dried blood spots.  
      关键词:bile acids;dried blood spots;LC-MS/MS;derivatization   
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    • WANG Qi, SU Jia-ting, YANG Hua-rui, ZHAO Yun-xia, XIAO Wei-min, YANG Guo-wu
      Vol. 44, Issue 5, Pages: 884-891(2025) DOI: 10.12452/j.fxcsxb.241009445
      Determination of Asparagine and Glutamine in Special Dietary Foods by Liquid Chromatography-Tandem Mass Spectrometry
      摘要:A liquid chromatography-tandem mass spectrometry method has been established for the determination of asparagine and glutamine in special dietary foods. Following the process of direct extraction or enzymatic extraction,the internal standard was added and the sample was separated by polar C18 chromatographic column(150 mm×4.6 mm,2.6 μm). The mobile phases consisted of acetonitrile and 0.02% formic acid in water. It was detected in a positive ion mode of electric spray for quantitative measurement and qualitative check. The results showed that there was a good linear relationship between asparagine and glutamine with correlation coefficients greater than 0.999. The linear range was 0-1 000 ng/mL. The limits of detection(LODs) were 0.8 mg/100g and 4.0 mg/100g for liquid and solid samples,respectively,and the limits of quantification(LOQs) were 2.4 mg/100g and 12 mg/100g for liquid and solid samples,respectively. The recoveries of the method ranged from 83.5% to 104%,with relative standard deviations ranging from 0.28% to 4.2%(n=6). This method has the advantages of simple pre-treatment,short analysis time,good accuracy,and high practicality. It can be used to precise quantification of asparagine and glutamine in specialty foods.  
      关键词:liquid chromatography-tandem mass spectrometry(LC-MS/MS);special dietary foods;asparagine;glutamine   
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      Experimental Techniques and Methods

    • LI Hui-qing, WANG Xu-feng, HOU Chao-ping, HUANG Ke, WANG Qiang
      Vol. 44, Issue 5, Pages: 892-898(2025) DOI: 10.12452/j.fxcsxb.241012458
      Determination of Mebendazole and Its Metabolites in Aquaculture Environments by Solid Phase Extraction and Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry
      摘要:In this study,an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of mebendazole and its two metabolites(amino-mebendazole and 5-hydroxymebendazole) in aquaculture water and sediment samples. The samples were extracted with ethyl acetate,and then purified with mixed-mode cation exchange(MCX) solid-phase extraction column. The targeted analytes were seperated on a Phenomenex Kinetex C18(100 mm×2.1 mm,2.6 μm) utilizing gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phases. Mebendazole and its metabolites were determined with positive electrospray ionization under multiple reaction monitoring mode,and quantified by internal standard method. The method showed good linearity in the range of 0.2-20 μg/L with correlation coefficients(r2) all above 0.998. The average recoveries in aquaculture water and sediment matrix were 85.6%-105%,with relative standard deviations(RSDs,n=6) of 3.4%-9.3%. The limits of detection for aquaculture water and sediment samples were 1.0-2.0 ng/L and 0.05-0.1 μg/kg,while the limits of quantitation were 2.0-5.0 ng/L and 0.1-0.2 μg/kg,respectively. The proposed method is sensitive and reliable,which can be applied to the determination of mebendazole and its metabolites in real aquaculture environment samples.  
      关键词:mebendazole;metabolite;solid phase extraction;aquaculture environment;ultra-performance liquid chromatography-tandem mass spectrometry   
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    • Research on Mass Spectrometry Signal Processing Based on EEMD-airPLS Method

      XIE Bin-rui, JU Zi-sheng, ZHAN Chen-rui, MA Qiang, LI Ming
      Vol. 44, Issue 5, Pages: 899-905(2025) DOI: 10.12452/j.fxcsxb.240924413
      Research on Mass Spectrometry Signal Processing Based on EEMD-airPLS Method
      摘要:The miniature mass spectrometer have become a hot research direction in the field of mass spectrometry,featuring direct on-site testing,rapid analysis speed,and strong portability. It has widespread applications in biomedical and food safety fields. However,due to factors such as sample pretreatment and the usage environment,issues like high signal noise and severe baseline drift often arise when handling complex matrices(e.g.,blood samples),significantly reducing the accuracy and stability of detection results in practical applications. The ensemble empirical mode decomposition(EEMD) method can adaptively decompose different physically meaningful characteristic components from the signals of miniature mass spectrometers,while the adaptive iteratively reweighted penalized least squares(airPLS) method can further process the background baseline of the signals. The combined use of these two methods can significantly improve the accuracy and stability of the signals. Using a miniature mass spectrometer,mass spectrometric signals of α-hydroxy pentanedioic acid and γ-aminobutyric acid were obtained from actual blood samples and processed with the EEMD-airPLS method,resulting in a significant improvement in the correlation coefficient(r²) and relative standard deviation(RSD),greatly enhancing the usability of data in actual blood sample testing. This approach provides a novel way for processing mass spectrometer signals,greatly expanding the application range of miniature mass spectrometers.  
      关键词:miniature mass spectrometer;signal analysis and processing;EEMD-airPLS method;blood samples   
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    • CHEN Zhi, FENG Ze-yang, ZENG Li-xi, ZHAO Jing, WANG Guang, ZHANG Na, XIE Yi-qiao
      Vol. 44, Issue 5, Pages: 906-912(2025) DOI: 10.12452/j.fxcsxb.240912393
      Study on the Determination of Polystyrene Microplastics in Whole Blood by PY/GC-MS and the Influence of Matrix Effects
      摘要:In order to investigate the matrix effect of microplastics in whole blood samples by pyrolysis gas chromatography-mass spectrometry(PY/GC-MS) and establish a quantitative method,this paper takes polystyrene microplastics as the research object,and uses three substrates and two pretreatment methods respectively to carry out group experiments. In order to find the optimal pretreatment method to reduce the influence of matrix effect. The results showed that there were significant matrix enhancement effects in different matrix supplemented samples. However,the matrix effect after pretreatment with potassium hydroxide(KOH) reagent was significantly weakened,and it was superior to the current mainstream enzymatic pretreatment results. This pretreatment method was significantly superior to enzyme method,easy to operate,and low reagent cost. It can be applied to the pretreatment of large quantities of samples and is currently the optimal pretreatment method. Finally,a quantitative method for determining polystyrene microplastics in whole blood samples using PY/GC-MS was established based on the optimized preprocessing method in this article. This method demonstrates a detection limit of 26 ng/mL and a quantification limit of 100 ng/mL,which can be used for practical applications. The research will have important reference value for the quantitative detection of microplastics in other biological matrices.  
      关键词:Py/GC-MS;polystyrene microplastics;quantitative analysis;matrix effect   
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    • LOU Feng-hua, HUANG Guo-pei, YANG Jun, TIAN Yi-fu, YU De-shun
      Vol. 44, Issue 5, Pages: 913-918(2025) DOI: 10.12452/j.fxcsxb.240901360
      Determination of Four Gingerol Compounds in Ginger by Supercritical Fluid Chromatography-Mass Spectrometry
      摘要:This study aimed to develop a new method to analyze 6-gingerol,8-gingerol,10-gingerol and 6-shogaol in ginger using supercritical fluid chromatography-mass spectrometry(SFC-MS). Separation was performed using an HSS C18 SB column(100 mm×2.1 mm,1.8 μm). Gradient elution was employed by the mixture of supercritical carbon dioxide and methanol with 0.2% formic acid as a modifier. The column temperature was 40 ℃,system back pressure was 13.79 MPa(2 000 psi) ,injection volume was 1 μL,and flow rate was 1 mL/min. Analytes were confirmed and analyzed using electrospray ionization(ESI) in positive ion and selected ion monitoring(SIR) modes,and quantified by external standard method. The results showed that the four target compounds were separated within 17 minutes,the correlation coefficients(r²) of the standard curves exceeded 0.995. The detection limits ranged from 0.05 to 0.08 µg/mL,and the quantification limits ranged from 0.5 to 0.8 µg/mL. The average recoveries of standard addition were between 84.1% and 105%,with relative standard deviations between 0.47% and 3.5%. The evaluation indicators demonstrated that the method had good precision and accuracy. The developed method was applied to ginger sample analysis and compared with high performance liquid chromatography(HPLC) method. The quantification results were comparable within the error range. The remarkable advantage of SFC-MS method was that the analysis time was less than half of HPLC method. In conclusion,SFC-MS method can be a novel analysis method for the rapid and efficient analysis of gingerols in ginger.  
      关键词:supercritical fluid chromatograph(SFC);mass spectrometry(MS);ginger;gingerol   
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    • LIU Ge, ZHANG Meng-wei, QIN Fang, CHEN Bin, CHEN Jun-sen, YANG Hao-zhang
      Vol. 44, Issue 5, Pages: 919-924(2025) DOI: 10.12452/j.fxcsxb.240915402
      Detection of Water Content in Transformer Oil Based on Infrared Spectroscopy
      摘要:The moisture content in transformer oil directly affects its electrical performance and may lead to safety hazards. Therefore,detecting moisture content is critical for ensuring the safe operation of transformers. By preparing oil samples with controlled moisture gradients and analyzing their infrared spectra,a multiple linear regression model correlating moisture content(W),absorbance at 3 400 cm-1(A),and absorption peak area(S) within 3 600-3 200 cm-1 was established. The model was validated using independent samples,proposing an accurate quantitative method for moisture detection via infrared spectroscopy. The results indicated that the absorption peaks in water-containing transformer oil arise from hydroxyl(—OH) vibrations in water molecules. Hydrogen bonding between water molecules and additives in the oil reduced the electron cloud density,leading to a redshift(lower wavenumbers) and broadening of the absorption peaks in the 3 600-3 200 cm-1 region. A quantitative model linking moisture content(W),absorbance at 3 400 cm-1(A),and absorption peak area(S) was established with high significance(R²=0.943,sig=0.003,p<0.05) and accuracy(RMSE=0.005 12). The experimental data points uniformly distributed on the regression plane confirm the model’s robustness in calculating moisture content. This method improves the accuracy of moisture quantification in transformer oil and provides a theoretical basis for future online monitoring systems.  
      关键词:infrared spectroscopy;transformer oil;moisture content;quantitative detection;multiple linear regression mathematical model   
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    • MA Hai-yu, LIAO Cai-yi, LIANG Qiu-yu, XIE Li-jun, LIU Lu-ying
      Vol. 44, Issue 5, Pages: 925-930(2025) DOI: 10.12452/j.fxcsxb.240811294
      A Ratiometric Fluorescent Sensor Based on the UiO-66-NH<sub>2</sub>@TCPP for the Detection of Arginine
      摘要:This study developed a ratiometric fluorescence sensor based on a fluorescence/colorimetric dual-mode approach by in situ encapsulating TCPP into UiO-66-NH₂ MOFs to form UiO-66-NH₂@TCPP for the detection of arginine. The fabricated sensor exhibited dual-emission characteristics under single-wavelength excitation at 360 nm,and the fluorescence intensity of UiO-66-NH₂ at 460 nm significantly increased with arginine concentration inereasing,while the emission peak of TCPP at 660 nm remained relatively stable. The result indicated that the ratio of F₄₆₀/F₆₆₀ demonstrated an excellent linear correlation with arginine concentrations in the range of 0.05-1.75 mmol/L and 1.75-6.0 mmol/L ,with a detection limit as low as 8.3 μmol/L. Compared to the single system of UiO-66-NH₂ MOFs,the ratiometric sensor had a lower detection limit and a wider detection range. Furthermore,the practical applicability of the sensor was successfully validated through spiked recovery tests in tap water and urine samples. Notably,the sensor could be adapted into a paper-based colorimetric platform for arginine detection. Under UV light irradiation,the UiO-66-NH₂@TCPP-loaded paper sensor displayed a visible color transition from red to blue upon exposure to arginine. Overall,this study offers a straightforward,convenient,and efficient strategy for on - site arginine detection.  
      关键词:MOFs;Ratiometric fluorescence sensor;UiO-66-NH2@TCPP;arginine   
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    • Research on Quantitation of DNA Based on Gel Electrophoresis Chip

      LI Zhen-qing, CHEN Qin, ZHU Jian-dong, ZENG Yuan, ZHANG Da-wei, Yamaguchi Yoshinori
      Vol. 44, Issue 5, Pages: 931-935(2025) DOI: 10.12452/j.fxcsxb.240911387
      Research on Quantitation of DNA Based on Gel Electrophoresis Chip
      摘要:To determine the DNA length and concentration of the bands after gel electrophoresis,this paper proposes an effective method to accurately analyze the length of DNA and its concentration by DNA fluorescence intensity from slab gel electrophoresis. Perform gel electrophoresis on the D2000 DNA ladder,collect image data,and process the images.The linear relationship between fluorescence intensity and DNA concentration,and the linear relationship between migration distance and DNA length were used for data analysis.Experimental results show that:When SYBR Green I was used as the fluorescent dye for electrophoresis of DNA,the green and red grey values in each pixel could reflect the characteristic information of DNA,and the green grayscale value was obviously higher than the red one. For the DNA fragments less than 2 000 bp,the migration distance were inversely proportional to the molecular weight,especially when the two value was calculated based on logarithmic,their correlation coefficient was 0.971,which could be used to establish a mathematical model for the calculation of DNA molecular weight based on its migration distance. By calculating the peak value and the peak area of the electropherogram,it was found that the ratios of the two DNA bands with the concentration ratio of 2∶1 were 2.16 and 1.96,2.11 and 1.94,2.16 and 1.93,indicating that the electrophoretic peak area was more effective in calculating the concentration value of DNA. This study has important application value for the development of nucleic acid gel electrophoresis instrument.  
      关键词:nucleic acid;gel electrophoresis;quantitative analysis;biochip   
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      Reviews

    • WANG Jia-min, GAO Xia
      Vol. 44, Issue 5, Pages: 936-946(2025) DOI: 10.12452/j.fxcsxb.241108516
      Advances in Microplastic Determination Technologies and Current Status of Domestic and International Standards
      摘要:Microplastics,as one of the important environmental issues worldwide,have become a key factor restricting the effective implementation of microplastic pollution regulation due to the insufficient standard system. The formulation and improvement of microplastic standard system are urgent. This paper aims to summarize the current development status of microplastic standards,provides an overview of commonly used determination methods for microplastics,and conduct in-depth comparative analysis of the differences and commonalities among different standards in defining the size range and composition of microplastics. The aim is to provide more accurate and consistent reference basis for the research,standardization,and supervision of microplastics,promote the standardization and unification of microplastic definitions,improve the microplastic standard system,and provide strong support for promoting the development of scientific research in the field of microplastics,as well as the supervision and governance of microplastic pollution problems.  
      关键词:microplastics;standards;composition;size   
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    • Progress in Electrochemical Detection of Silver Ions

      WU Di, CHEN Song-min, XU Wen-hui, ZHANG Xi-yao, HU Qiong, YANG Song-lin, NIU Li
      Vol. 44, Issue 5, Pages: 947-955(2025) DOI: 10.12452/j.fxcsxb.240819325
      Progress in Electrochemical Detection of Silver Ions
      摘要:Given the widespread use of silver in daily life and industry and,in particular,the detrimental effects of silver ions (Ag+) in the environment on living organisms,the quantitative assay of Ag+ is of great importance to life and health,drinking water safety,environmental monitoring,etc. Relative to other methods,electrochemical sensors have attracted much more attention in Ag+ detection due to the advantages of fast response,simple instrumentation,easy miniaturization,low cost,high sensitivity,wide measurement range,and good portability. In this review,the progress in Ag+ detection using the voltammetric,potentiometric,and impedimetric sensors are summarized,with a focus on their detection principles (including electrode materials) and analytical performance. Also,the challenges with respect to the practical applications of electrochemical sensors in Ag+ detection are mentioned and the further development of electrochemical Ag+ sensors is prospected.  
      关键词:electrochemical analysis;electrochemical sensor;Ag+ detection;electrochemical detection   
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    • PAN Yan-fang, LI Xiao-jing, YANG Wen-chao, LI Dong, LIAO Hua-ping, XU Yan-na
      Vol. 44, Issue 5, Pages: 956-967(2025) DOI: 10.12452/j.fxcsxb.240905374
      Application of X-ray Photoelectron Spectroscopy in Chemical State Analysis of Transition Metal Compounds and Rare Earth Compounds
      摘要:X-ray photoelectron spectroscopy(XPS) is an important method for surface chemical states analysis,which has been widely used in various fields of scientific research and has greatly promoted the development of scientific research. However,the chemical state analysis for the transition metal compounds and rare earth compounds are difficult because of their complex structure,multiple splitting and broadening of the spectral peaks. In this paper,the chemical state analysis methods are summarized by introducing the standard spectra of transition metal compounds and rare earth compounds in database or handbook,which are peak fitting method,characteristic satellite peak judgment method,and kinetic energy of Auger line or modified Auger parameter method,etc. The calculation of modified Auger parameters is presented. For rare earth compounds,there are few databases and standard narrow spectra that can be referred to,the spectral peaks are extremely complex,and many elemental and combined states have unique peaks,which make it more difficult to analyze,this paper takes La and Ce as examples. For the analysis of mixed valence states,the nonlinear least square fitting method(NLLSF) is introduced,which is a method to build a preset peak shape function based on the real spectrum function. The energy loss peak,satellite peak and multiple splitting peak are all included in the spectrum,which can accurately fit the peak shape,and is simple,convenient and reliable for dealing with the spectrum of mixed chemical states coexistence. There are overlap between Ni 2p and F KLL,among Ni,Co,Mn and Fe,and the anode target are suggested to replace to make the Auger lines move and separate from the main photoelectron peak,which will make it much more convenient for the subsequent data analysis. Querying whether there is a standard spectrum in the database website for reference before data analysis is important,and for those elements without a standard narrow spectrum to refer to,objective,reasonable and self-consistent analysis should be carried out in combination with the narrow spectrum of other elements and the qualitative and semi-quantitative results of the sample,avoiding analyzing by experimental expectations or speculative inferences.  
      关键词:X-ray photoelectron spectroscopy(XPS);chemical state analysis;mixed chemical state analysis;modified Auger parameter;non-linear-least square fitting(NLLSF);transition metal compounds;rare earth metal compounds   
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    • Research on the Quality Evaluation Method System of Graphene Products

      LI Mao-dong, WEN Fang, WANG Liang-wang, HE Li-liang
      Vol. 44, Issue 5, Pages: 968-976(2025) DOI: 10.12452/j.fxcsxb.240815308
      Research on the Quality Evaluation Method System of Graphene Products
      摘要:With the innovation and upgrading of large-scale preparation of graphene materials,advanced technology of graphene,and industrial application of graphene materials in China,it is particularly important to study and form graphene measurement standards,quality evaluation methods and application criteria with wide applicability and strong universality. In this paper,the market status of graphene materials and products were introduced,and the progress of graphene standardization research was reviewed. The evaluation method system of graphene product quality was analyzed from four aspects,including:the detection method based on different forms of graphene,the detection method based on carbon materials and graphene-like materials,the detection method based on characterization means,and the detection method based on the graphene application field. Finally,the opportunities and challenges of graphene detection are summarized,and the possible development direction in the future is prospected.  
      关键词:graphene;detection method;quality evaluation;standardization;architectural research   
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    • WANG Jing, LIU Shuang-yi, JIN Zhi-lin, XIAO Xue, LU Qiao
      Vol. 44, Issue 5, Pages: 977-984(2025) DOI: 10.12452/j.fxcsxb.240920408
      摘要:Catecholamines(CAs) and its metabolites are bioactive substances that play an important role in bodies. Abnormally elevated levels of adrenaline and norepinephrine often indicate the presence of adrenal tumors or pheochromocytomas. Their metabolites methoxyprenophrine and nomethoxyprenophrine are important biomarkers for detecting paraganglioma and pheochromocytoma,while imbalances of dopamine and its metabolites are associated with neurological disorders such as Parkinson's disease. Liquid chromatography-tandem mass spectrometry(LC-MS/MS) has become one of the preferred methods in the field of small molecule biomarker detection due to its high sensitivity,high specificity and wide linear range. However,it still has disadvantages,such as high cost,high technical requirements and tedious sample pretreatment. This paper reviews the research progress of LC-MS/MS in the detection of CAs and their metabolites,including its detection process,clinical application and main problems,and the prospect of the future detection of CAs by LC-MS/MS technology was discussed.  
      关键词:LC-MS/MS;catecholamine;metabolites;sample pretreatment;quantitative analysis   
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