最新刊期
      卷 42 ， 期 3 ， 2023

        Scientific Papers

      • CHEN Hai-jie,ZHOU Yong-yi,XUE Jia,ZOU Li-si,WU Nan,YUAN Jia-huan,LIU Xun-hong,YANG Wei,CHENG Jian-ming
        Vol. 42, Issue 3, Pages: 251-263(2023) DOI: 10.19969/j.fxcsxb.22120602
        摘要：An ultra-fast liquid chromatography－triple quadrupole－linear ion trap mass spectrometry（UFLC－QTRAP－MS/MS） was developed for the rapid and simultaneous analysis of 60 active constituents including flavonoids，tannins，phenolic acids，nucleosides，polyphenols and amino acids in Tetrastigmae Radix，which was combined with multivariate statistical analysis to evaluate the quality of Tetrastigmae Radix dried or processed by different methods．The gradient separation was performed on an XBridge®C18 column（4.6 mm × 100 mm，3.5 µm） with 0.4% formic acid－methanol as mobile phase，and the mass spectrometric detection was carried out in electrospray positive or negative ion mode under multiple reaction monitoring（MRM） mode. The samples of differently dried and processed Tetrastigmae Radix were comprehensively evaluated by entropy weight TOPSIS，analysis of variance（ANOVA） method and gray correlation analysis（GRA） according to the contents of 60 target constituents．The results showed that there were good linear relationships for 60 target constituents in a certain mass concentration range，with their correlation coefficients（r2） not less than 0.999 0．The limits of detection（LODs） and the limits of quantitation（LOQs） were in the range of 0.03－13.59 ng/mL and 0.09－45.30 ng/mL，respectively．The average spiked recoveries for the samples ranged from 96.1% to 102%，with relative standard deviations（RSDs） less than 5%．Different drying methods have certain effects on the multiple active constituents in Tetrastigmae Radix，and modern drying methods could significantly retain the active constituents in Tetrastigmae Radix compared with the traditional drying methods．The ANOVA showed that the low temperature drying treatment had a good retention effect on flavonoids，tannins，and polyphenols．The loss of nucleosides and phenolic acids in Tetrastigmae Radix was low under vacuum drying conditions．Sun-drying or shade-drying treatment tends to cause the loss of amino acids in Tetrastigmae Radix．The results of GRA and TOPSIS analyses were the same，and the quality ranking of each group was the same，indicating that different drying methods had significant effects on the active constituents in Tetrastigmae Radix，with large differences between groups．GRA and TOPSIS analyses both indicated that the comprehensive quality of Tetrastigmae Radix samples treated by vacuum drying was better，while the overall quality of Tetrastigmae Radix treated by freeze-drying，hot-air drying，sun-drying，and shade-drying was relatively poor．TOPSIS was more suitable than GRA for distinguishing the quality of Tetrastigmae Radix samples．The comprehensive analysis showed that the comprehensive quality of the vacuum-drying treated Tetrastigmae Radix was better under the five drying and processing methods．The method developed in this study is accurate and stable，which could provide an experimental basis for the rational drying and processing of Tetrastigmae Radix，and also provide a new method reference for the comprehensive evaluation and overall control of the quality of Tetrastigmae Radix herb.  
        关键词：Tetrastigmae Radix;different drying methods;multiple active constituents;multivariate statistical analysis;ultra-fast liquid chromatography－triple quadrupole－linear ion trap mass spectrometry（UFLC－QTRAP－MS/MS）   
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        发布时间：2023-04-17
      • RONG Yu-tang,ZHANG Xian-chen,DENG Xiao-ying,WU Jie-shan,LIU Qiong-yu,CAI Jie,WENG Fu-liang
        Vol. 42, Issue 3, Pages: 264-274(2023) DOI: 10.19969/j.fxcsxb.22102903
        摘要：An ultra performance liquid chromatography－quadrupole/exactive orbitrap mass spectrometry（UPLC－Q Exactive Orbitrap MS） with dispersive liquid－liquid microextraction（DLLME） was established for the simultaneous determination of 139 drug residues in 5 categories，including antibiotics，hormones，prohibited dyes，pesticides and mycotoxins．The influences of various conditions on the extraction effect of DLLME were investigated．The optimal extraction conditions were as follows：5.0 g of sampling volume，50 µL of extraction agent tetrachloroethane，300 μL of dispersant acetonitrile，0.30 g of sodium chloride and 8 min of ultrasonic time．After extraction，the samples were separated on a Shimadzu Shim-pack XR－ODS II（150 mm × 2.0 mm，2.2 µm） column．By using Q－Exactive Orbitrap MS to determine the intensity of the exact mass number of precursor ion in full scan，quantitation on multi-type targets could be realized．Combined with retention time and data-dependent MS/MS（DD－MS2） scanning，the precise mass numbers of the fragment ions could be determined，followed by rapid confirmation and screening with MS/MS spectral library．The results showed that there were good linear relationships for the peak intensities of 139 compounds in mass concentration ranges of 10－1 000 ng/mL（r > 0.99）．The detection limits were 10－30 µg/kg，and the recoveries were 63.0%－95.9%，with relative standard deviations（RSDs） between 3.0% and 9.5%．The deviations for each accurate mass number were less than 3 × 10-6．This method is stable，simple，rapid，accurate，low consumption of organic reagents and environmentally friendly，and it is suitable for rapid screening of lotion.  
        关键词：dispersive liquid－liquid microextraction;ultra performance liquid chromatography－quadrupole/exactive orbitrap mass spectrometry;lotion;drug residues   
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        发布时间：2023-04-17
      • RU Li-hua,LÜ Wei,WANG Xiang-qi,ZHANG Zhi-juan
        Vol. 42, Issue 3, Pages: 275-282(2023) DOI: 10.19969/j.fxcsxb.22111401
        摘要：A gas chromatography－mass spectrometry（GC－MS） was adopted to detect the breath samples of 180 subjects in this paper，including 79 patients with lung cancer and 101 healthy controls. A total of 92 volatile organic compounds（VOCs） were detected. Furthermore，10 potential characteristic VOCs for lung cancer patients were screened out by orthogonal partial least－squares discrimination analysis（OPLS－DA） model combined with Mann－Whitney test，including benzaldehyde，cis-2-butene，2-butanone，naphthalene，vinyl acetate，ethylene，2，2，4-trimethylpentane，3-methylpentane，hexanal and 2-methylpentane. Thereafter，the metabolic differences in different populations and possible related metabolic mechanisms were analyzed using statistical method. Then，the diagnostic performance of candidate breath VOC biomarkers for lung cancer were verified by establishing machine learning models. The results showed that，the diagnostic accuracy，precision，sensitivity and specificity of random forests were 96.25%，96.21%，95.76% and 96.67%，respectively，and the Matthews correlation coefficient（MCC） was 0.93，the area under ROC curve was 0.96. All the 10 compounds could be taken as the potential breath VOC biomarkers for discriminating lung cancer and health people，which have supplied rich basic data for early diagnosis of lung cancer.  
        关键词：lung cancer;volatile organic compounds;breath biomarkers;diagnosis model;gas chromatography－mass spectrometry   
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        发布时间：2023-04-17
      • ZHOU Ya-ru,HAO Rong,WU Yu-peng,HE Chen,SHI Quan,HU Rong-gui
        Vol. 42, Issue 3, Pages: 283-291(2023) DOI: 10.19969/j.fxcsxb.22111504
        摘要：Fourier transform－ion cyclotron resonance mass spectrometry（FT－ICR MS） was applied to the analysis of the molecular structure characteristics of dissolved organic matter（DOM） in soil and water of Danjiangkou Reservoir in this paper．The compound type distribution，equivalent double bond number and carbon number distribution of soil and aquatic DOM were obtained．The results showed that the soil DOM was composed of 6 classes of compounds，i.e. CHO，CHOS1，CHON1，CHON2，CHON3 and CHON1S1，of which the CHO class was the most abundant，and the major part of this class was lignin．Meanwhile，the aromatic structures of soil DOM were mainly related to CHO and CHON1 class compounds．The molecules with low and high oxygen atoms were likely to contain aromatic structures，while the constituent of aquatic DOM was similar to that of soil，but the ratio of each class among 6 classes was different between both of them．The major parts of CHO class species of aquatic DOM were also lignin．Aromatic structure was also mainly related to CHO and CHON1 class compounds．The molecules with low oxygen atoms were likely to contain branched chain structures，while the molecules of oxygen atoms from 4 to 19 contain more carboxyl and aromatic structures．This study provided convincing evidence for better understanding the DOM molecular structure from different ecosystems．  
        关键词：dissolved organic matter;soil;water;Fourier transform－ion cyclotron resonance mass spectrometry（FT－ICR MS）   
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        发布时间：2023-04-17
      • YAN Zhi-qi,WANG Jie,WANG Hui,WANG Fu-hua,ZHANG Li-jun,TAN Yin-xiang,WU Ri-wei,HUANG Wen-jie,HUANG Zao-tian,TAN Guo-bin
        Vol. 42, Issue 3, Pages: 292-298(2023) DOI: 10.19969/j.fxcsxb.22111701
        摘要：A novel and rapid detection system for trace components in indoor air of passenger vehicles was developed，based on the independently developed vacuum ultraviolet single photon ionization time-of-flight mass spectrometer and on-line high precision formaldehyde analyzer．Firstly，the indoor air of passenger vehicles was replaced by purified air，then the trace components of volatile organic compounds in indoor air of passenger vehicles were continuously detected with volatile organic compounds online mass spectrometer，while the formaldehyde in indoor air of passenger vehicles was continuously detected by using an online high precision formaldehyde analyzer．The results indicated that benzene，toluene，xylene/ethylbenzene，styrene and formaldehyde exhibited good linearity in the corresponding concentration ranges，with their correlation coefficients（r2） all greater than 0.99，and relative standard deviations less than 5%．The limits of detection were 1.3 × 10-9，0.1 × 10-9，0.2 × 10-9，0.8 × 10-9 and 0.1 × 10-9 mol/mol，respectively．This method was applied to determine the indoor air of passenger vehicles．The results showed that the VOCs in indoor air of passenger vehicles could be released quickly to reach a sub-equilibrium state in a short time，and the results of VOCs concentration and release rate under the sub-equilibrium state could be obtained．The concentrations of benzene，toluene，xylene/ethylbenzene，styrene and formaldehyde in indoor air of the tested vehicle were 0.30，8.90，25.10，21.90 and 15.05 µg/m3，respectively．With no complex and time-consuming sampling process and easy to operate，this proposed method could meet the requirements for rapid detection and screening on the trace components in indoor air of passenger vehicles.  
        关键词：passenger vehicles;indoor air;trace components of VOCs;rapid detection   
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        发布时间：2023-04-17
      • FENG Jun-jun,WANG Jing,ZHAO Lian-xing,JIANG Hai-yun,LIAN Ya-lin,TAN Tian-yu,ZHANG Fan,JING Zheng-yi,HE Feng,LI Teng-fei
        Vol. 42, Issue 3, Pages: 299-306(2023) DOI: 10.19969/j.fxcsxb.22110801
        摘要：A new type of solid phase extraction column filler metal organic frame material（MOFs） UiO－66－NH2 was prepared，and a solid phase extraction/high performance liquid chromatography－tandem mass spectrometry（SPE/HPLC－MS/MS） was developed for the determination of new red in beverages and prepared wines. The structure and adsorption properties of UiO－66－NH2 were characterized by scanning electron microscopy，infrared spectroscopy and nitrogen adsorption－desorption isotherm. The samples were separated on a Waters AtlantisTM T3（150 mm × 2.1 mm，3 μm） column with 10 mmol/L ammonium acetate aqueous solution and methanol as mobile phases，and analyzed in multiple reaction monitoring（MRM） mode. The results showed that，under the optimal extraction conditions，the calibration curves for new red showed good linearities in the range of 0.05－10 mg/L， with correlation coefficients（r2） of 0.998.The limits of detection（LODs） and limits of quantitation（LOQs） were 0.05 mg/L and 0.15 mg/L，respectively. The recoveries of this method ranged from 87.8% to 107%， with relative standard deviations（RSDs，n = 6） of 1.9%－11%， indicating that this method has good accuracy and precision. It is also proved that the UiO－66－NH2 based solid phase extraction column could be used as a high quality adsorption material for detection of new red in beverages and prepared wines.  
        关键词：metal organic frameworks;solid phase extraction;high performance liquid chromatography－tandem mass spectrometry;new red;beverage;prepared wines   
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        发布时间：2023-04-17
      • LIANG Xiao-juan,WANG Ya-ni,MA Jin-fang,SUN Peng,GUO Tuo,YAN Shi-kai,XIAO Xue
        Vol. 42, Issue 3, Pages: 307-314(2023) DOI: 10.19969/j.fxcsxb.22102901
        摘要：A qualitative analysis method based on sparse principal component analysis feature selection（SPCAFS） and support vector machine（SVM） modeling was proposed in this paper，in order to realize the rapid discrimination on the origin of Crataegi Folium. Near infrared integrative sphere diffuse reflection spectroscopy was used to collect the near-infrared spectrograms of 123 Crataegi Folium samples from 6 regions in 41 batches. After data preprocessing，the representative characteristic bands were selected by SPCAFS，and the near infrared origin discrimination model for Crataegi Folium was established by SVM. The model was compared with three feature selection algorithms，i.e. continuous projection algorithm（SPA），regularized self representation algorithm（RSR） and sparse subspace clustering（SSC），to evaluate the prediction performance of the proposed model with accuracy，precision and sensitivity as evaluation criteria. The results showed that the numbers of characteristic band for SPCAFS were reduced from 1 500 to 21 compared with those for full wavelength modeling，but the accuracy and precision of prediction results were improved from 78% and 76% to 97% and 100%，respectively. Meanwhile，compared with those of SPA，RSR and SSC algorithms，the accuracy was improved by 6%，3% and 3%，while the precision was improved by 13%，10% and 5%，respectively. The prediction ability of the model was significantly improved. The SVM discrimination model based on SPCAFS could realize the rapid discrimination on the northern and southern geographic origins of Crataegi Folium.  
        关键词：near infrared spectroscopy;feature selection;Crataegi Folium;geographic origin discrimination;sparse principal component analysis for feature selection;support vector machines   
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        发布时间：2023-04-17
      • YIN Xue-hu,YANG Xin-jie,LUO Dan,ZHANG Yan-li,WANG Hong-bin,YANG Wen-rong,PANG Peng-fei
        Vol. 42, Issue 3, Pages: 315-322(2023) DOI: 10.19969/j.fxcsxb.22110703
        摘要：Hollow porous gold nanoparticles（HPAuNPs） were prepared by a simple solution phase sacrificial template method．The hollow porous gold nanoparticles/reduced graphene oxide（HPAuNPs/rGO） nanocomposite was prepared for the effective immobilization of glucose oxidase（GOx） on the surface of glassy carbon electrode（GCE）．An electrochemical biosensor for detection of glucose was constructed based on GOx/HPAuNPs/rGO modified GCE．Scanning and transmission electron microscopy，X-ray photoelectron spectroscopy，X-ray diffraction spectroscopy，infrared spectroscopy and electrochemistry were used to characterize the morphology and structure of the nanomaterial，the immobilization process of GOx，and the direct electrochemical behaviors and the electrocatalytic properties of the biosensor．The results showed that the HPAuNPs/rGO nanocomposite could effectively accelerate the direct electron transfer（DET） between GOx and electrode due to the synergy effect of HPAuNPs and rGO．The modified electrode exhibited an excellent electrocatalytic property for glucose determination．The response current was proportional to the concentration of glucose in the range of 0.05－7.0 mmol/L，with a detection limit（S/N = 3） of 16 μmol/L．With good selectivity，reproducibility and stability，the proposed biosensor could satisfy the demands for glucose detection in real serum sample，with recoveries of 98.0%－103%，and relative standard deviations（RSDs） not more than 5.0%.  
        关键词：glucose oxidase;hollow porous gold nanoparticles;reduced graphene oxide;electrochemical biosensor   
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        发布时间：2023-04-17
      • CHEN Bin,ZHENG Xiao-huan,GENG De-chun,QI Wen-liang,LU Dao-li
        Vol. 42, Issue 3, Pages: 323-329(2023) DOI: 10.19969/j.fxcsxb.22101601
        摘要：7 standard substances and 26 mixtures made from 7 standard substances were selected as the research objects in this paper， with the accuracy and misjudgment rate as the evaluation indexes for recognition effect of the components of mixtures， and spectral peak matching algorithm， non-negative least squares matching algorithm and correlation coefficient matching coefficient algorithm were studied， in order to solve the problem of identifying the components of mixtures. Furthermore， a BP neural network model infrared spectroscopy technique based on multi-feature fusion was used to identify the components of the mixture， which was compared with the logistic regression model. The results showed that the recognition accuracies of three single matching algorithms are lower than 76.31%， while the recognition accuracies of multi-feature fusion logistic regression model and multi-feature fusion BP neural network model prediction set are 83.33% and 98.18%， respectively， and the misjudgment rates are 4.76% and 1.82%. The results showed that mid-infrared spectroscopy combined with BP neural network model could better identify the components of the mixture. In order to further explore the detection ability of the model towards the lowest concentration of mixed components， the detection limit for vanillin and ethanol solution was studied. The results showed that the accuracy rate was 100.00% and the misjudgment rate was 14.29% when the concentration of vanillin was 0.03 g/mL. When the concentration of vanillin was lower than 0.03 g/mL， the accuracy decreased by 20.00% and the misjudgment rate increased by 19.04%. Therefore， it may be considered that the minimum mass concentration of vanillin in vanillin and ethanol solution identified in this study is 0.03 g/mL.  
        关键词：infrared spectroscopy;mixture;multi-parameters;BP neural network;component identification   
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        发布时间：2023-04-17
      • YIN Yan-yan,YANG Jun-lin,TIAN Dong-wei,JIANG Li-li,YOU Xiao-long,ZHANG Jian,CHENG Ping-yan
        Vol. 42, Issue 3, Pages: 330-336(2023) DOI: 10.19969/j.fxcsxb.22091503
        摘要：An ultra-high performance liquid chromatography－high resolution mass spectrometry（UPLC－HRMS） was established for the determination of 19 amino acids in Baijiu．The samples were firstly removed ethanol by oven-drying method，then the volume was fixed with ultrapure water，and filtered using an aqueous phase filter membrane before analysis．The samples were separated on a Hypersil GOLD column（150 mm × 2.1 mm，1.9 μm） with methanol－0.1% formic acid solution as mobile phase．The data were collected in full mass scan in positive ESI mode and the external standard method was used to achieve quantitative analysis．The results showed that the calibration curves for 19 amino acids showed good linear relationships within corresponding linear range，with correlation coefficients（r2） not less than 0.986 2．The limits of detection and the limits of quantitation were in the range of 0.003－0.015 μmol/L and 0.008－0.050 μmol/L，respectively．The recoveries for Baijiu samples ranged from 88.2% to 119%，with relative standard deviations of 0.23%－5.6%．This method was suitable for the determination of amino acids in Baijiu samples．The contents of amino acids in different rounds base liquor of sauce-flavor Baijiu were analyzed by this method．Sixteen amino acids，i.e. L-alanine，L-arginine，L-aspartic acid，L-glutamic acid，glycine，L-histidine，L-isoleucine，L-leucine，L-lysine，L-phenylalanine，L-proline，L-serine，L-threonine，L-tyrosine，L-valine and L-citrulline were detected．The significant level P values of amino acid contents in different rounds base liquor of sauce-flavor Baijiu were all less than 0.05，indicating that amino acid contents in different rounds base liquor had significant differences.  
        关键词：amino acids;Baijiu;ultra-high performance liquid chromatography－high resolution mass spectrometry（UPLC－HRMS）   
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        发布时间：2023-04-17

        Experimental Techniques and Methods

      • WANG Xu-feng,WANG Qiang,ZHANG Ying-xia,HUANG Ke
        Vol. 42, Issue 3, Pages: 337-343(2023) DOI: 10.19969/j.fxcsxb.22102501
        摘要：A multi-residue analytical method was developed for the simultaneous determination of diazepam and its three metabolites in aquaculture water and sediment samples based on ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）．Water samples were filtered through 0.45 μm glass fiber membranes，and subsequently enriched with a mixed cation exchange solid phase extraction（MCX SPE） cartridge．Sediment samples were extracted with 1% ammonium hydroxide－ethyl acetate，and then cleaned up using a MCX SPE cartridge．The purified extracts were eluted with 5% ammonium hydroxide－acetonitrile solution，and then dried residues were redissolved with 1 mL 40% acetonitrile water solution for UPLC－MS/MS analysis．The chromatographic separation of four targeted analytes were performed on a Phenomenex Kinetex C18（100 mm × 2.1 mm，1.7 μm） column by gradient elution，with acetonitrile and 0.1% formic acid solution as mobile phases．Targeted compounds were determined with positive electrospray ionization under multiple reaction monitoring（MRM） mode，and quantified by internal standard method．Good linear relationships for targeted analytes were obtained in the range of 0.1－100 μg/L with correlation coefficients（r2） larger than 0.999．The detection limits of the method for aquaculture water samples and sediment samples were 1.0－2.0 ng/L and 0.02－0.05 μg/kg，while the quantitation limits were 2.0－5.0 ng/L and 0.05－0.1 μg/kg，respectively．The average recoveries for spiked negative aquaculture water and spiked sediment matrix ranged from 90.2% to 115%，with relative standard deviations（RSDs，n = 6） between 2.1% and 9.6%．The proposed method is sensitive and accurate，and it is suitable for the residual determination of diazepam and its metabolites in real aquaculture water and sediment samples.  
        关键词：diazepam;metabolite;solid phase extraction（SPE）;ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）;aquaculture environment   
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        发布时间：2023-04-17
      • WANG Meng-ru,YIN Yao,NING Xiao-pan,ZHANG Ping,PENG Jun,LOU Yun,DING Tao,WU Li-na,LIU Han,ZHANG Xiao-yan
        Vol. 42, Issue 3, Pages: 344-350(2023) DOI: 10.19969/j.fxcsxb.22103101
        摘要：An analytical method was developed for the simultaneous determination of ethoxyquinoline and ethoxyquinoline dimer residues in aquatic products such as fishes，shrimps，loaches and crabs by high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）．An appropriate amount of vitamin C was added in the sample preparation．Acetonitrile was used as the extraction solvent，and hexane was used for liquid－liquid extraction．The supernatant was cleaned up on an Oasis PRiME HLB solid-phase extraction column and spun to near dryness，acetonitrile was used to fix the volume．Then the sample was separated on an Agela Phenomenex Kinetex C18 column（100 mm ×4.6 mm × 2.6 μm），and subsequently detected with electrospray ionization source in positive ionization mode under selected reaction monitoring（SRM） mode，and quantified by external standard method. There were good linear relationships for both ethoxyquinoline and ethoxyquinoline dimer in concentration range of 1－100 μg/L，with their correlation coefficients（r2） greater than 0.994. The limits of detection（LODs） and limits of quantitation（LOQs） of the method were 0.5 μg/kg and 1.5 μg/kg，respectively. The average recoveries for two target substances at four spiked levels of 1.5，5，10 and 100 μg/kg ranged from 75.8% to 103%，with relative standard deviations（RSDs） of 0.58%－9.6%. The developed method is sensitive，accurate and precise，and it could be applied to the determination of ethoxyquinoline and ethoxyquinoline dimer in aquatic products such as fishes，shrimps，loaches and crabs.  
        关键词：high performance liquid chromatography－tandem mass spectrometry;aquatic products;ethoxyquinoline;ethoxyquinoline dimer;solid-phase extraction   
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        发布时间：2023-04-17
      • LI Jia-shuai,XUE Lian-lian,WANG Kai,LIU Jun-cheng,WU Han,LI Hua-qing,YIN Feng-fu
        Vol. 42, Issue 3, Pages: 351-356(2023) DOI: 10.19969/j.fxcsxb.22101104
        摘要：In order to identify different types of plastics，the near-infrared spectral data of four types of plastics，i.e．nylon（PA），polypropylene（PP），polystyrene（PS） and polyvinyl chloride（PVC），were collected．Meanwhile，according to the existing noise，baseline and optical path issues during spectral data acquisition，pretreatment combination optimization methods were investigated，based on 3-point Savitzky－Golay convolution smoothing（S－G），first derivative（FD），second derivative（SD），standard normal variable transformation（SNV） and multivariate scattering correction（MSC）．Furthermore，the characteristic wavelength was extracted by competitive adaptive reweighting sampling（CARS），and a model was established using support vector machine（SVM）．The results showed that among all preprocessing methods，the preprocessing combination S－G + FD + SNV obtains the best results，while the average accuracy of the S－G + FD + SNV + SVM model is as high as 96.67%，and the average accuracies of its training set and validation set are both 100%．The mentioned-above pretreatment combination optimization method could provide a reference for the identification on four common plastics.  
        关键词：plastic sorting;near-infrared spectroscopy（NIR）;preprocessing;combination;predictive analysis   
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        发布时间：2023-04-17
      • ZAN Yan-nan,ZHANG Xiao-yun,SHANG Shao-hua,CHEN Ning,DING Yi-mei
        Vol. 42, Issue 3, Pages: 357-362(2023) DOI: 10.19969/j.fxcsxb.22091201
        摘要：A method based on liquid－liquid extraction（LLE）/gas chromatography－mass spectrometry（GC－MS） was developed for the determination of 16 phthalate plasticizers（PAEs） in the extracts of plastic components used in the production of fludeoxyglucose［18F］ injection. According to the production process，the simulated solvent for extraction experiments was a mixture of 5% ethanol and 5% acetonitrile，and the extraction temperature was simulated at 40 ℃. The extracts were separated on a Thermo TG－5 SIL MS column，and analyzed in selected ion scanning mode（SIM）. The instrument conditions and the extraction conditions were optimized to determine the most suitable pre-treatment method and instrument conditions. Under the optimized experimental conditions，the peak areas of 16 PAEs were linearly correlated in the range of 50－500 ng/mL，with correlation coefficients（r） not less than 0.990 6. The limits of detection（LODs） and limits of quantitation（LOQs） were 10 ng/mL and 30 ng/mL，respectively. The average recoveries ranged from 83.0% to 114% with relative standard deviations（RSDs，n = 6） of 1.9%－4.2% when dichloromethane was used as the extraction solvent. 16 PAEs did not exceed the analytical evaluation threshold（AET） when the extracts were determined by this method. The method is simple and specific，and it could be used to study the compatibility of plastic production components for fludeoxyglucose ［18F］ injection.  
        关键词：gas chromatography－mass spectrometry;liquid－liquid extraction;plasticizers;fludeoxyglucose ［18F］ injection;plastic components   
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        发布时间：2023-04-17
      • LIU Man,ZHAO Tian,LIU Hui-li,CHEN Lin
        Vol. 42, Issue 3, Pages: 363-367(2023) DOI: 10.19969/j.fxcsxb.22111901
        摘要：A quantitative proton nuclear magnetic resonance（qHNMR） method was developed for determination on the effective content of tofacitinib citrate tablets，with dimethyl sulfoxide（DMSO－D6） as the solvent and 3，5-dimethylpyrazole as the internal standard．Proton signal peaks of tofacitinib at δ 7.13 and δ 5.73 of 3，5-dimethylpyrazole were selected as the quantitative signals，respectively．The spectra of the mixture complex were collected under the conditions of pulse sequence zg30，relaxation delay time（D1） 26 s，and scanning number（NS） 16 times at 298 K on Bruker Avance Ⅲ 400 MHz NMR spectrometer．qHNMR method with high specificity showed a good linear relationship in the concentration range of 0.793－7.925 mg/mL，with linear correlation coefficient（r2） up to 0.998 4．The relative standard deviation（RSD） of precision，repeatability and stability were 0.82%，1.7% and 0.67%，respectively．The content of tofacitinib in tofacitinib citrate tablets was determined to be 2.25% by qHNMR，which was basically consistent with the results by high performance liquid chromatography（HPLC）．As a result，qHNMR method is an alternative way to determine the effective content of toacitinib cittrate tables．More importantly，it has many outstanding advantages，such as simple operation，short detection time，no requirement for reference standards，simultaneously qualitative and quantitative analysis.  
        关键词：quantitative proton nuclear magnetic resonance（qHNMR）;tofacitinib citrate tablets;3，5-dimethylpyrazole;content determination   
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        发布时间：2023-04-17

        Review

      • HAN Wen-hao,LI Yan-sheng,GAO Guo-wei,ZHANG Xue-ji
        Vol. 42, Issue 3, Pages: 368-374(2023) DOI: 10.19969/j.fxcsxb.22101402
        摘要：Aflatoxin B1（AFB1） has strong toxicity and carcinogenicity，and its dose exceeding the standard will seriously endanger the health of organisms．The development of new AFB1 detection methods is of great significance for the prevention and control of its harm．The traditional method for AFB1 detection is mature and reliable，with low detection limit，but relying on professional equipment and professionals．It cannot meet the needs of on-site detection．Aptamer biosensors have the advantages of high sensitivity，high specificity and simple operation，which have attracted attention in the detection of AFB1．Meanwhile，researchers have developed many new methods based on different principles．The related properties of AFB1 and its traditional detection methods are firstly introduced in this paper，and then the construction of aptamer biosensors based on optical，electrochemical and microfluidic chips in recent years as well as their applications in the field of AFB1 detection are summarized．It provides a reference for the development of practical application of aptamer biosensors，and discusses the development prospects and future trends of aptamer biosensors by discussing the problems in the currently developed detection methods.  
        关键词：aflatoxin B1;aptamer;biosensor;application   
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