最新刊期
      卷 42 ， 期 2 ， 2023

        Scientific Papers

      • SONG Zhong-rong,ZHOU Xiang,JIANG Qing-xiang,YAN Zhi-hong,CAI Ying,LI Hui
        Vol. 42, Issue 2, Pages: 131-140(2023) DOI: 10.19969/j.fxcsxb.22101704
        摘要：A gas chromatography－mass spectrometry with magnetic solid phase extraction based on Fe3O4@SiO2@NH2@C60 magnetic nanocomposites was established for the simultaneous determination of 16 polycyclic aromatic hydrocarbons（PAHs） in Chinese herbal medicines in this paper．The composites were characterized by Fourier transform infrared spectroscopy，scanning electron microscopy and vibrating sample magnetometer to confirm the successful modification of C60．Meanwhile，adsorption experiments were conducted，which showed that the magnetic nanocomposites had a strong adsorption capacity and good stability，and the adsorption efficiency did not change significantly after 10 times of reuse．The effects of extraction solvent type，sorbent dosage，adsorption time，desorption solvent type and desorption time on the extraction efficiency for 16 PAHs in herbal samples were investigated．The results showed that the complete adsorption of 10 mg of sorbent on the targets could be achieved within 4 min．Under the optimal magnetic solid phase extraction conditions，there were good linear relationships for 16 PAHs in the range of 5－1 000 µg/L，with correlation coefficients（r2） of 0.994 0－0.999 9．The limits of detection and the limits of quantitation were in the range of 0.2－1.2 µg/kg and 0.8－3.9 µg/kg，respectively．The spiked recoveries at three levels ranged from 84.1% to 104%，with relative standard deviations（RSDs） of 0.70%－8.3%，intra-day RSDs of 0.20%－3.5% and inter-day RSDs of 2.2%－6.9%．The developed method could effectively reduce the interference on PAHs targets from complex matrices in Chinese herbal medicine samples，and provide an easy-to-operate，sensitive and accurate method reference for the determination of PAHs in Chinese herbal medicines.  
        关键词：polycyclic aromatic hydrocarbons;magnetic nanospheres;C60;magnetic solid phase extraction/gas chromatography－mass spectrometry;Chinese herbal medicines   
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        发布时间：2023-02-28
      • WANG Tian-shan,FU Zi-zhuo,JIANG Fang-long
        Vol. 42, Issue 2, Pages: 141-149(2023) DOI: 10.19969/j.fxcsxb.22091303
        摘要：Tandem mass spectrometry（MS/MS） generates fragmentation ions from quasi-molecular ions．Meanwhile，high-resolution mass spectrometry offers an accurate mass measurement，which is particularly suitable for the analysis of fragmentation pathways and structure identification of natural products．In this paper，fifteen natural compounds of Euphorbia diterpenoid，classified as myrsinane-type（1－9） and pemyrsinane-type（10－15） possessing chemical structural features of 5/7/6/3 and 5/7/6 ring fused system，were selected to analyze the basis of characteristic MS/MS fragmentation patterns．Experimental data indicated that diterpenoid backbone fragments were yielded by continuous acids，carboxylates elimination and dehydration upon higher-energy collision dissociation（HCD）．Compounds 1－7 fragmented to yield backbone ions of m/z 311（ion A） and m/z 293（ion B），compounds 8 and 9 gave at m/z 295（ion C） and m/z 277（ion D），and similarly，compounds 10－15 showed them at m/z 313（ion E） and m/z 295（ion F）．A series of diagnostic ions including backbone ions in the low mass region of m/z 200－320 were identified，which were associated with specific structural features．The neutral losses of H2O，HCHO，CO，C3H4 and/or acetone were the characteristic eliminations from the backbone precursor ions due to the presence of hydroxyl，THF（tetrahydrofuran） ring，carbonyl，isopropenyl and/or CH3C（OH）CH3 units in the structures．The occurrence of key diagnostic ions and their fragmentation patterns could potentially permit the chemical structure determination and the identification for unknowns.  
        关键词：Euphorbia diterpenoid;myrsinane-type;premyrsinane-type;fragmentation pattern;diagnostic ions   
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        发布时间：2023-02-28
      • CHEN Fang-ru,ZHANG Zhao-kang,HE Shu-han,YU Xi-xi,LI Yan-xia
        Vol. 42, Issue 2, Pages: 150-157(2023) DOI: 10.19969/j.fxcsxb.22082503
        摘要：Glucose level is an important evaluation index for the diagnosis and treatment of diabetes．In this paper，a novel portable glucose sensor was constructed based on laser-induced graphene/enzyme electrodes.Micro-flexible graphene three-electrode system（LIG electrode） was prepared by laser-induced graphene（LIG） technique．The effect of π－π superposition occurred between the hydrophobic terminal benzene ring of 1-pyrene butyric acid and the six-membered ring structure of graphene introduced the carboxyl onto the LIG electrode，then the glucose oxidase（GOx） was covalently cross-linked to the surface of LIG for preparation of LIG/GOx electrodes．Glucose sensing was carried out by chronoamperometry．Results showed that the constructed sensor could be used to detect glucose in the range of 5.0 × 10-5－1.0 × 10-2 mol/L with a limit of detectton（S/N = 2） of 5.0 × 10-5 mol/L．The method showed high selectivity，stability and good reusability，and could be used to detect glucose in serum，urine and sweat samples．LIG is a micro-electrode material for glucose sensing with good development prospects，which is conducive to the realization of non-clinical glucose detection and is expected to be used in the construction of portable sensors.  
        关键词：laser induced graphene;glucose;electrochemical analysis;biosensor   
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        发布时间：2023-02-28
      • JIE Zhao-wei,ZHOU Shi-rui,WANG Ji-fen,KONG Yi-qing,LI Wen-ping,SHAO Zuo-shan
        Vol. 42, Issue 2, Pages: 158-165(2023) DOI: 10.19969/j.fxcsxb.22091602
        摘要：A rice seed pattern recognition method based on terahertz time-domain spectroscopy was proposed in this paper in order to crack down on illegal elements peddling unqualified rice seeds in qualified seeds to obtain illegal profits．Compared with traditional methods，the terahertz time-domain spectroscopy was fast，time-saving and non-destructive，which could meet the needs of front-line law enforcement personnel for rapid detection of samples．In the experiment，10 kinds of rice seeds containing mixed adulteration of different brands were selected as samples，and the terahertz time-domain spectral data of the samples were collected．Meanwhile，relief，random forest（RF），support vector machine recursive feature elimination（SVM－RFE） and maximum relation minimum redundancy（mRMR） models were established to select the spectral wavelengths of the samples，respectively．Finally，a classifier was designed to classify and identify the samples processed by the four feature selection methods．The experimental results showed that the extreme learning machine（ELM） model optimized based on the cuckoo search（CS） algorithm had the best recognition effect on the sample spectral data extracted by the random forest feature selection algorithm，with an accuracy reaching 100%．The experiment is of a certain reference significance for the identification of seed adulteration in the field of forensic science.  
        关键词：terahertz time-domain spectroscopy;pattern recognition;rice seeds;feature selection;adulteration identification   
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        发布时间：2023-02-28
      • LIN Yong-jian,XU Dun-ming,SHEN Lu-ying,LIU Zheng-cai,LI Yu-zhe,WANG Wei,XIAO Jing
        Vol. 42, Issue 2, Pages: 166-172(2023) DOI: 10.19969/j.fxcsxb.22090101
        摘要：A development method for nicarbazin residue matrix reference materials in chicken muscle was established in this paper to fill the gap of those in China．Positive animals with nicarbazin residues were obtained by feeding white feather broiler chickens with nicarbazin drug powder in feed and allowing the drug to metabolize naturally in the chickens．A batch of 355 chicken lyophilized powders containing nicarbazin residues were prepared by taking chicken breast meat and making minced meat，through the processes of homogenization，freeze-drying，crushing，sieving，packaging and irradiation sterilization．Homogeneity assessments，stability monitoring，characterization and uncertainty analysis were carried out according to the requirements of national reference materials．The contents of nicarbazin in the samples were determined by liquid chromatography－tandem mass spectrometry（LC－MS），which were cooperatively certified by 8 expert laboratories．The results showed that the homogeneity and stability of this batch of reference materials were good and they could be kept stable for 14 days under the temperature conditions of -70 ℃，4 ℃，25 ℃ and 50 ℃，and up to 12 months when stored at -18 ℃，which was in accordance with the relevant requirements of the national reference materials．The certified value of nicarbazin in the reference materials was finally determined to be （157.7 ± 11.0） μg·kg-1（k = 2）．The reference material could be used for optimization of detection methods for nicarbazin，and capacity evaluation on nicarbazin residue testing laboratories，which is of great significance to the detection of nicarbazin residues in food.  
        关键词：chicken;nicarbazin;matrix reference material;liquid chromatography－tandem mass spectrometry（LC－MS/MS）   
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        发布时间：2023-02-28
      • YANG Shan-yi,CHEN Hong-wei,ZHOU Hai-lin,ZHU Yi-fan,ZHANG Jia-hao,WANG Xuan-cheng,HUANG Zong-sheng,ZHANG Qi-song
        Vol. 42, Issue 2, Pages: 173-180(2023) DOI: 10.19969/j.fxcsxb.22092103
        摘要：Colorectal cancer（CRC） is one of the most vital causes of cancer-related death worldwide，while colorectal adenoma（CA） is an important precancerous lesion of CRC. The development of a CA into a CRC is a relatively long and stealthy process．However，there is still a lack of minimally invasive and reliable biomarkers to distinguish CA from CRC．In this paper，an ultrahigh-performance liquid chromatography－tandem high-resolution mass spectrometry（UHPLC－HRMS） combined with multivariate statistical analysis was used to analyze the untargeted metabolomics of serum samples from 64 CA patients and 84 CRC patients．The acquired metabolomics data were analyzed by unsupervised segregation principal component analysis（PCA） to visualize the grouping trends and detect outliers．A supervised orthogonal partial least squares discriminant analysis（OPLS－DA） was subsequently utilized to maximize the discrimination between the groups．The established OPLS－DA model was validated by 200 times of permutation tests to confirm its rationality and reliability in data analysis．Then the serum differential metabolites responsible for the discrimination between the groups were screened based on the criteria of P < 0.05 and fold change > 1.50 or < 0.67，and further identified using the mzCloud and HMDB databases．The discriminative ability for differential metabolites was verified by receiver operating characteristic（ROC） analysis．Moreover，the pathway and enrichment analyses of differential metabolites using MetaboAnalyst were used to preliminarily explore the metabolic mechanism of CA cancerization．Results showed that there were certain differences in serum metabolic profiles between the two groups，and 66 differential metabolites were screened and identified，including glycerophospholipids，fatty acids，sphingomyelins，steroids，amino acids，nucleosides and cholines．These differential metabolites mainly involved in the biosynthesis of unsaturated fatty acids，purine metabolism and linoleic acid metabolism，suggesting that they may be closely related to the carcinogenesis of CA．11 metabolic biomarkers including adenine，PC18∶0，arachidonic acid，docosahexaenoic acid，PC 36∶3，8，11，14-eicosatrienoic acid，PC 20∶4，SM d36∶2，5，8，11，14，17-eicosapentaenoic acid，sphingosine（d18∶1），and ACar 20∶1 showed good specificity and sensitivity with the area under the ROC curves greater than 0.80，which had the strong discriminant ability and high potential in clinical application to distinguish CA and CRC．Especially，the area under the ROC curve of the marker panel including PC 36∶3，adenine，sphingosine，PC 18∶0，and PC 20∶4 was 0.941，which presented an outstanding discriminant performance on the CA and CRC．The marker panel discovered provides a valuable reference for the early prevention of CRC clinically.  
        关键词：colorectal cancer;colorectal adenoma;ultrahigh-performance liquid chromatography－tandem high-resolution mass spectrometry（UHPLC－HRMS）;serum metabolomics;biomarkers   
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        发布时间：2023-02-28
      • LI Jing,YAN Meng,SHEN Jin-can,XIAO Chen-gui,MAK Yim-ling,LI Yang,GUO Jian-ning,ZHONG Run-sheng
        Vol. 42, Issue 2, Pages: 181-188(2023) DOI: 10.19969/j.fxcsxb.22081704
        摘要：A method was established for the simultaneous detection of 18 marine phycotoxins by ultrahigh performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） combined with solid phase extraction，including azaspiracids（AZAs），brevetoxins（BTXs），Pacific ciguatoxins（P－CTXs），dinophysistoxins（DTXs），gymnodimine（GYM），maitotoxin3（MTX3），okadaic acid（OA），pectenotoxin2（PTX2），spirolide1（SPX1） and yessotoxins（YTXs） etc．Seawater（1 L） or the ultrasonic extracts of suspended particulate matter or sediment（1 g） was extracted with solid phase extraction cartridges（Agilent Bond Elut C18，500 mg/6 mL），and then 10% glycerol－methanol was added to the eluent to reduce the loss of target toxins．Water was the aqueous phase and 95% acetonitrile/water was the organic phase，both of which contained 0.1% formic acid and 2 mmol/L ammonium formate．A Phenomenex Kinetex C18 column（100 mm × 2.1 mm i.d.，1.7 μm） was used to separate the phycotoxins in six minutes，and then the target analytes were detected by UPLC－MS/MS in multiple reaction monitoring mode．The external standard method was used for the quantitation of 18 phycotoxins．The correlation coefficients of standard curves were 0.991 1－0.999 9．The quantitation limits of the methed for 18 phycotoxins ranged from 0.05 to 250 pg/L（or pg/g）．The matrix-spiked recoveries for 18 phycotoxins ranged from 77.4% to 119%，with the relative standard deviations of 1.1%－15%．Ten phycotoxins were detected in seawater from the Pearl River Estuary，with the predominant PTX2 of 36.6－7 900 pg/L．MTX3 concentrations ranging from 0 to 262 pg/L was monitored for the first time．With good sensitivity and precision，this method can satisfy the requirements for simultaneous determination of 18 phycotoxins in seawater，suspended particulate matter and sediment.  
        关键词：ultrahigh performance liquid chromatography－tandem mass spectrometry;solid phase extraction;phycotoxins;seawater;suspended particulate matter;sediment   
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        发布时间：2023-02-28
      • YANG Jian-ying,ZHU Hong,XU Ning,CHEN Xiao-hong,CHEN Qing,XIAO Heng
        Vol. 42, Issue 2, Pages: 189-196(2023) DOI: 10.19969/j.fxcsxb.22092203
        摘要：A QuEChERS/high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） was established for the rapid and simultaneous determination of 21 anesthetics in skin care products．The samples were dispersed with water，then extracted with acetonitrile solution containing 1.0%（by volume） formic acid by ultrasound extraction，and purified with anhydrous magnesium sulfate，octadecyl silane（C18） and primary secondary amine（PSA），and finally seperated on an Acclaim Mixed－Mode WCX－1 column（150 mm × 2.1 mm，3 μm） which could offer multiple retention mechanisms including reversed-phase（RP），weak cation-exchange（WCX） and HILIC．The mobile phases were 20 mmol·L-1 ammonium formate（adjusting to pH 4.0） and acetonitrile（cantaining 0.035% formic acid）．The samples were detected in electrospray positive ion mode under multiple reaction monitoring（MRM） mode，and quantified by matrix-matched standard solutions and external standard method．There were good linear relationships for 21 anesthetics in the concentration range of 0.5－100 ng·mL-1，with their correlation coefficients（r） larger than 0.99．The detection limits and quantitation limits were 0.1－3 μg·kg-1 and 0.3－10 μg·kg-1，respectively．The average recoveries at three spiked levels for the 21 analytes in three matrices ranged from 84.3% to 109%，with relative standard deviations of 0.70%－7.1%（n = 6）．The method is simple to operate，and it is suitable for the daily detection of 21 anesthetics in skin care products.  
        关键词：QuEChERS;high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）;anesthetic;skin care product   
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        发布时间：2023-02-28
      • LIU Zhen,WANG Yu-mei,HU Wen-yan
        Vol. 42, Issue 2, Pages: 197-203(2023) DOI: 10.19969/j.fxcsxb.22103102
        摘要：A high performance liquid chromatography－tandem mass spectrometric（HPLC－MS/MS） method was developed for the determination of five peptide antibiotics，i.e．daptomycin，vancomycin，norvancomycin，virginiamycin M1 and virginiamycin S1 in pork based on a purification technique with non-activation pass-through solid phase extraction（SPE） column．The pork samples were extracted with methanol－2% formic acid（5∶2，by volume），and purified with a non-activation Captiva EMR－Lipid SPE column．The separation was carried out on a Phenomenex Kinetex F5（2.1 mm × 100 mm，2.6 μm） column by gradient elution，with 0.1% formic acid acetonitrile solution and 0.1% formic acid as mobile phases．The target substances were analyzed in electrospray ion source positive ion mode under multi-reaction monitoring（MRM） mode，and quantified by the internal standard method．Results showed that the calibration curves of five peptide antibiotics in pork were linear（r2 > 0.99） in the range of 2－200 ng/mL for daptomycin，5－500 ng/mL for vancomycin and norvancomycin，and 1－100 ng/mL for virginiamycin M1 and virginiamycin S1．The limits of detection were in the range of 3－7.5 μg/kg，and the limits of quantitation were in the range of 5－25 μg/kg．The recoveries of five peptide antibiotics from negative pork samples at three spiked levels of 25，50，250 μg/kg ranged from 80.2% to 102%，with intra-RSDs and inter-RSDs of 1.3%－7.4% and 2.6%－8.5%，respectively．With the characteristics of simple pretreatment，good recovery and repeatability，this method based on Captiva EMR-lipid SPE column is suitable for the simultaneous analysis of 5 peptide antibiotics in pork.  
        关键词：peptide antibiotics;liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）;pork;pass-through solid phase extraction   
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        发布时间：2023-02-28

        Experimental Techniques and Methods

      • ZHANG Zhan-ge,NI Li-jun,ZHANG Li-guo,LUAN Shao-rong
        Vol. 42, Issue 2, Pages: 204-209(2023) DOI: 10.19969/j.fxcsxb.22101501
        摘要：Previous studies have shown that selecting suitable wavelengths to establish a near-infrared（NIR） spectral model can realize the transfer of calibration model without standard samples．Using the corn spectra of three near-infrared instruments and the protein in corn as the case study，a two-step wavelength selection method of MC－UVE－VIP is proposed in this paper by combining Monte Carlo-uninformative variable elimination（MC－UVE） method with variable importance in projection（VIP） method．The method selects important and informative wavelength variables to build partial least square（PLS） calibration model for protein in corn．Firstly，the method uses MC－UVE to screen the set of UUVE consisting of informative wavelengths，whose stability parameter for screening wavelengths are greater than a threshold（Mthreshold）．Then，the VIP algorithm is used to screen the important and informative wavelength set of UUVE-VIP，whose VIP parameter is greater than the average value of VIP of all wavelengths in the UUVE．A PLS near-infrared spectral model for predicting protein in corn is established based on UUVE-VIP．The number of latent variables of the PLS model is determined according to the principle that accumulative contribution rate of the first latent variables should be higher or equal to 99.9%．The model is of few variables，robust，good at interpretability，and fast at calculation．The mean absolute relative error（MARE） of predicting protein in the samples tested on the secondaries is 1.64% and 1.88%，respectively．While the MARE of the secondary samples predicted by MC－UVE and VIP models are 5.19%－5.40% and 6.23%－7.16%，respectively．Therefore，the near-infrared spectral model of corn protein based on the MC－UVE－VIP two-step wavelength screening method can be directly transferred to the secondary instruments without correcting model or secondary samples spectra．The transfer performance of the model is better than that of the model based on single MC－UVE or single VIP wavelength selection algorithm，and is better than full wavelength model．The adoptability of the two-step wavelength selection method of MC-UVE－VIP for the other data set needs to be inspected further.  
        关键词：two-step wavelength screening;Monte Carlo-uninformative variable elimination（MC－UVE）;variable importance in projection（VIP）;model transfer without standard samples;prediction of corn protein   
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        发布时间：2023-02-28
      • MA Ling,MA Qian,LI Ya-jiao,ZHANG Yi-yang,WANG Jing,MA Si-yan,MA Yan,DU Ming-hua,WU Long-guo
        Vol. 42, Issue 2, Pages: 210-215(2023) DOI: 10.19969/j.fxcsxb.22083102
        摘要：A near infrared hyperspectral imaging（NIR） technique was adopted for qualitative identification on the tomato leaves under different salt stress in order to quickly monitor the growth of tomato plants．The average spectral reflectance data of 192 leaf samples were collected．The original spectral data were preprocessed by multiple scattering correction（MSC），standardized normal variate（SNV），orthogonal signal correction（OSC） and correlation optimized warping（COW） to establish a partial least squares regression（PLSR） model．The modeling results showed that the modeling effect of OSC preprocessed spectrum was the best．Interval variable iterative space shrinking analysis（iVISSA），interval random frog（IRF），genetic algorithm and partial least squares（GAPLS），competitive adaptive weighted sampling（CARS） and variable combination population analysis（VCPA） were used to extract the feature wavelengths，thus the PLSR model was established．The results showed that the model established by VCPA extracting characteristic wavelengths was optimal．The VCPA method was used to extract 11 characteristic wavelengths（945，975，990，1 002，1 005，1 067，1 204，1 326，1 595，1 642，1 660 nm），which were used to establish the qualitative discriminant prediction model for tomato leaves，while the determination coefficient（RP2） of the optimal prediction model and the root mean square error（RMSEP） were 0.917 and 0.456，respectively．This study provided a technical support for online monitoring of plant growth in the future.  
        关键词：hyperspectral imaging technique;tomato leaves;salt stress;nondestructive testing   
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        发布时间：2023-02-28
      • KONG De-ming,CHEN Chao,ZHOU Qi-dong,LIU Ze-hua,GUO Peng-ran
        Vol. 42, Issue 2, Pages: 216-220(2023) DOI: 10.19969/j.fxcsxb.22063007
        摘要：Natural estrogens are a class of endogenous hormones，but their exogenous intake may still be harmful to human health．Milk is one of the significant sources of exogenous natural estrogens in humans．Therefore，accurate analysis of natural estrogen in milk is an important prerequisite for evaluating its exogenous intake．In this paper，a gas chromatography－mass spectrometric（GC－MS） method was developed for the simultaneous determination of six natural estrogens in milk，including estrone（E1），17α-estradiol（17α-E2），17β-estradiol（E2），estriol（E3），16α-hydroxyl estrone（16αOHE1） and 16ketoestradiol（16ketoE2）．Milk samples were extracted with acetonitrile，enriched and purified with a OASIS HLB Cartridge in turn，then derivatized with BSTFA+1% TMCS．The results showed that six estrogens had good linear relationships in the concentration range of 5－100 µg/L，with correlation coefficients（r2） larger than 0.995．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.17－0.51 µg/L and 0.56－1.68 µg/L，respectively．The average recoveries ranged from 83.1% to 119%，with relative standard deviations（RSDs，n = 9） of 2.1%－15%．The method was applied to the detection of natural estrogens in actual milk samples，and all the estrogens compounds were detected in except E3，indicating that 16αOHE1 and 16ketoE2 should not be ignored．With good accuracy and precision，this method is suitable for the detection of natural estrogens in milk.  
        关键词：milk;natural estrogens;gas chromatography－mass spectrometry（GC－MS）;liquid liquid extraction;solid phase extraction   
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        发布时间：2023-02-28
      • XU Ai-li,CAO Ying-nan,ZHANG Su-zhong,QIU Jin-yan,XIE Can-hui,BI Xiao-li,XIAO Guan-lin
        Vol. 42, Issue 2, Pages: 221-226(2023) DOI: 10.19969/j.fxcsxb.22101102
        摘要：An ultra performance liquid chromatography（UPLC） coupled with evaporative light scattering detection（ELSD） was established for the simultaneous determination of 5 saponins，i.e．polyphyllin I，polyphyllin Ⅱ，polyphyllin Ⅶ，saikosaponin a and saikosaponin d in Chonglou Xiaoliu Formula. The samples were extracted with methanol， then separated on a Waters Cortecs UPLC C18（150 mm × 2.1 mm，1.6 μm） column with acetonitrile－water as the mobile phase by gradient elution，finally determined by ELSD and quantified by external standard calibration method．The results showed that there were good linear relationships for 5 saponins in the ranges of 7.117 4－177.94 μg/mL，9.407 2－235.18 μg/mL，8.872 6－221.82 μg/mL，7.486 2－187.15 μg/mL and 9.761 3－244.03 μg/mL，respectively，with their correlation coefficients（r） of 0.999 2－0.999 8．The limits of detection and the limits of quantitation were in the ranges of 0.7－1.0 μg/mL and 1.8－2.4 μg/mL，respectively．The average recoveries were 93.9%，103%，102%，104% and 105%，with their relative standard deviations（RSDs） of 3.8%，4.0%，4.2%，3.6% and 3.2%，respectively．With the advantages of simplicity，rapidness and accuracy，the method could be applied in simultaneous analysis of 5 saponins in Chonglou Xiaoliu Formula and effective elimination of the impurity interference．And it also provides a reference for the quality evaluation on Chonglou Xiaoliu Formula．  
        关键词：Chonglou Xiaoliu Formula;saponins;ultra performance liquid chromatography;evaporative light scattering detection   
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        发布时间：2023-02-28
      • LIU Yang,CHEN Shao-zhan,LIU Li-ping,LI Xiao-yu,LI Qian-yu
        Vol. 42, Issue 2, Pages: 227-232(2023) DOI: 10.19969/j.fxcsxb.22091504
        摘要：A high performance liquid chromatography－inductively coupled plasma mass spectrometry（HPLC－ICP－MS） was developed for the analysis of six arsenic speciations，i.e．arsenic betaine（AsB），dimethyl arsenic（DMA），arsenic choline（AsC），arsenite（As（Ⅲ）），monomethyl arsenic（MMA） and arsenate（As（V）） in human urine．After the samples were diluted with water，the arsenic speciations were separated on a Dionex IonPac As7 anion exchange column by gradient elution，with 20 mmol/L ammonium carbonate（2% methanol） and 100 mmol/L ammonium carbonate（2% methanol） as the mobile phase，and finally analyzed by HPLC－ICP－MS．The results indicated that the linear ranges for six arsenic speciations were all between 0 μg/L and 100 μg/L，with their correlation coefficients（r） more than 0.999．The detection limits were between 0.05 μg/L and 0.15 μg/L．The reproducibility of this method was evaluated by precision under different concentrations，with relative standard deviations（RSDs） less than 5.0%．The recoveries for six arsenic speciations at three spiked levels ranged from 91.8% to 108%．The evaluation results for five arsenic speciations in the standard reference material－Arsenic Species in Frozen Human Urine（NIST SRM 3669） were all within the range of standard values．This method was sensitive，rapid，reproducible and accurate，and it was suitable for rapid determination of arsenic speciations in human urine．The arsenic species in human urine were also characterized after food consumption．It was revealed that different metabolic transformations occurred in human body after different foods containing arsenic were consumed.  
        关键词：urine;arsenic speciation;high performance liquid chromatography－inductively coupled plasma mass spectrometry   
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        Reviews

      • ZHANG Guang-teng,HE Hong-yuan,HUANG Jia-dong,ZHOU Zong-xian
        Vol. 42, Issue 2, Pages: 233-240(2023) DOI: 10.19969/j.fxcsxb.22100401
        摘要：New psychoactive substances（NPSs） have been proliferating in recent years，posing a threat to public health and social stability through contributing to social issues like crime．NPSs are quickly metabolized in the human body，while mass spectrometry could be used to effectively determine a substance’s ingestion by detecting its distinctive metabolites．The in vitro and in vivo metabolic studies of NPSs in the last five years are reviewed in this paper by searching，organizing，and discussing the pertinent literature．The applicability，benefits and drawbacks of various methods are also summarized and compared to data from real human samples．Finally，the development trend of metabolic research methods is looked ahead with a view to providing references for metabolic studies of NPSs such as metabolite identification and metabolite inference.  
        关键词：new psychoactive substance;metabolism;mass spectrometry;review   
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      • ZHOU Shu-wei,FU Hong,YANG Fang
        Vol. 42, Issue 2, Pages: 241-250(2023) DOI: 10.19969/j.fxcsxb.22092602
        摘要：The issue of pesticide residues in food is of great concern．The extraction and purification of food matrices by sample pretreatment techniques are necessary for the complex matrixes of food products containing many types of pesticides and very small amounts．In the sample pretreatment process，sorbent materials play an important role．In recent years，magnetic carbon materials（mCBMs） have received much attention in the field of pesticide residue analysis in food due to their good purification effect，rapid separation and easy recovery．In this paper，the preparation of magnetic graphene，magnetic carbon nanotubes，magnetic graphitized carbon black and their modification with functional groups，polymer and functional materials are introduced．The application and the problems and future prospects of mCBMs in the detection of pesticide residues in food are outlined．It is anticipated to provide a reference for expanding the application of mCBMs in the detection of pesticide residues.  
        关键词：pesticide residues;magnetic carbon materials;food;preparation;modified;detection and analysis   
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