最新刊期
      卷 42 ， 期 6 ， 2023

        Scientific Papers

      • ZHOU Min,WU You-yi,YU Qin,WEI Wei
        Vol. 42, Issue 6, Pages: 657-665(2023) DOI: 10.19969/j.fxcsxb.23031802
        摘要：A high performance liquid chromatography（HPLC） with dispersive liquid－liquid microextraction was developed for the detection of antifungal drugs，including ketoconazole，clotrimazole，terbinafine and econazole in environmental samples，based on the solidification of floating natural deep eutectic solvent（SFNADES） wihic was newly synthesized with lauric acid as the hydrogen bond donor and 1-octanol as the hydrogen bond acceptor．The extraction conditions，including extractant type and molar ratio，extractant volume，sample volume，sample pH value，ionic strength，vortex time and centrifugation time were optimized to obtain the best extraction efficiency．Under the optimal conditions，the linear ranges of four antifungal drugs（r2 ≥ 0.999 8） ranged from 0.56 μg/L to 500 μg/L，with limits of detection（LODs） of 0.17－0.80 μg/L，limits of quantitation（LOQs） of 0.56－2.67 μg/L，and enrichment factors of 101－114．The intra-day and inter-day realtive standard deviations（RSDs，n = 6） were lower than 4.8% and 5.4%，respectively．The method was successfully applied to the detection of four antifungal drugs in real water and human urine samples with recoveries of 91.5%－107%.  
        关键词：natural deep eutectic solvent（NADES）;dispersive liquid－liquid microextraction;antifungal drugs;lauric acid;environmental samples   
        80
        |
        28
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706001 false
        发布时间：2023-06-15
      • SHI Xiao-na,LIN Jia-wei,YIN Yi,ZHENG Guang-ming,JIN Hui,LIU Xue-wen,ZHAO Cheng,SHAN Qi
        Vol. 42, Issue 6, Pages: 666-673(2023) DOI: 10.19969/j.fxcsxb.23010802
        摘要：A magnetic porous carbon material Fe@Fe3C－C was prepared by derivatizing an iron-based metal organic framework MIL－88B（Fe） in this paper，and applied to the efficient adsorption of bisphenol A（BPA） in water．The crystal structure，morphology and surface area of the material were characterized by X-ray diffraction，scanning electron microscopy，surface area and pore size analysis. The results showed that MIL－88B（Fe） was transformed into Fe and Fe3C co-doped carbon material（Fe@Fe3C－C） under high temperature，which had a layered burst-like sheet structure with rough surface．The specific surface area of Fe@Fe3C－C was 280.48 m2/g，17 times higher than that of MIL－88B（Fe）．The adsorption experiment showed that，compared with MIL－88B（Fe），calcination at high temperature（≥ 600 ℃） could improve the adsorption performance significantly．The removal rate of BPA of 10 mg/L reached 95% within 10 min when the amount of Fe@Fe3C－C was 0.5 g/L．The material had a wide range of pH application（pH 2.0－10.0） and a strong ability against ionic interference（100 mmol/L），and was suitable for BPA adsorption in high-salt environment．The pseudo-second-order kinetic model accords with the adsorption kinetics curve for BPA on Fe@Fe3C－C，and the adsorption process accords with the Langmuir model．Cyclic experiments showed that Fe@Fe3C－C has a good recycling ability and could be easily recovered from water．X-ray photoelectron spectroscopy and zeta potential were used to investigate the adsorption mechanism．The main mechanisms of Fe@Fe3C－C were π－π interaction，charge interaction and micropore filling．These results indicated that Fe@Fe3C－C has a great application potential in the removal of BPA in water.  
        关键词：MIL－88B（Fe）;carbon derivatization;BPA;adsorption   
        31
        |
        6
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706075 false
        发布时间：2023-06-15
      • SHI You-zhi,PAN Yong,DU Fu,ZHAO Ze-yu,LI Zi-wei,WANG Yan-yan,YUAN Xiao-long,ZHANG Zhong-feng,PANG Xue-li,WANG Jian
        Vol. 42, Issue 6, Pages: 674-683(2023) DOI: 10.19969/j.fxcsxb.22113001
        摘要：To clarify the flavor characteristics of different species of cigar leaves，a static headspace/gas chromatography－ion mobility spectrometry（SHS/GC－IMS） was applied to the comparative analysis of volatile composition in five kinds of superior cigar leaves，including three domestic and two foreign varieties．Then，the flavor characteristics of different cigar leaves were evaluated based on calculation of odor activity value（OAV）．Consequently，the differential odorant markers among different cigar leaves were screened based on multivariate statistical analysis of their OAVs．A total of 82 volatile flavor compounds were detected and identified in domestic and foreign cigar leaves，covering a wide range of 11 chemical categories，including nitrogen-contained compounds（amines，pyridine，pyrazine and nitriles），oxygen-contained heterocyclic compounds，sulfur-contained compounds，aliphatic alcohols，aliphatic aldehydes，aliphatic ketones，aliphatic acids，aliphatic esters，lactones，monoterpenes and aromatic compounds．Among these identified volatile compounds，trimethylamine dominated both in concentration and OAV in all cigar leaves．Therefore，it was deemed to be the main source of the pungent ammonia and fishy odor of cigar leaves．Hierarchical cluster analysis（HCA） showed that in terms of volatile components，Chuxue 80 and Chuxue 81 were similar to Dominican cigar leaves．They were characterized by rich aroma properties，dominated by “creamy”，and supplemented by “cocoa-like/roasted/nutty” and “spicy” note．While the flavor of Indonesian cigar leaves was unique，with the “fruity-sweet” as the most prominent flavor attribute．The partial least squares discriminant analysis（PLS－DA） based on OAVs showed that trimethylamine（ammonia/fishy），ethyl 3-methylbutyrate（apple/citrus/sweet），2，3-butanedione（butter/cream），ethyl isobutyrate（apple/tropical fruit），dimethyl disulfide（cabbage/earth/sulfide），1-penten-3-ol（mushroom/earth），2-methylpropanal（dark chocolate），hexal（grassy），ethyl butyrate（apple/banana），ethyl acetate（fruity），2-methyl propanoic（cheesy） were the main odorant markers responsible for flavor differences among all cigar leaves．The results of present research could provide data support and theoretical guidance for improving the flavor quality of domestic cigar tobacco leaves and developing the flavor-guided production technology for cigar leaves.  
        关键词：cigar leaves;volatile flavor compounds;static headspace/gas chromatography－ion mobility spectrometry;multivariate statistical analysis;odor activity value;differential odorant marker   
        31
        |
        10
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705841 false
        发布时间：2023-06-15
      • LIU Fu-bang,WANG Ji-fen,ZHANG Ying
        Vol. 42, Issue 6, Pages: 684-691(2023) DOI: 10.19969/j.fxcsxb.23022204
        摘要：As the variety of new psychoactive substances（NPS） continues to increase and their abuse becomes more and more widespread，their rising popularity poses a serious challenge to national anti-drug agencies．Herein，a direct analysis of real time－tandem mass spectrometry（DART－MS/MS） was developed for the detection of 12 NPS of benzodiazepines（DBZDs） in urine．The MS conditions，including injection volume，carrier gas heater temperature and pretreatment method were optimized．Methodological validation was performed．The results showed that the best pretreatment effect was obtained by liquid-liquid extraction using ethyl acetate．Then，5 µL supernatant was pipetted into the bottom of a glass rod，and a DART 12Dip－It™ sampler was used for sampling．The best response was obtained by analysis in positive ionization mode under multiple reaction monitoring（MRM） mode at a carrier gas heater temperature of 300 ℃．The quantitation analysis of DBZDs was performed by internal standard method with diazepam-D5 as the internal standard．The linear relationships for 12 DBZDs were good in the range of 0.05－5 μg/mL，with correlation coefficients（r2） great than 0.99．The limits of detection and the limits of quantitation were in the range of 0.5－20 ng/mL and 1－50 ng/mL，respectively．The average matrix effects were in the range of -11.1%－12.6%．The average recoveries ranged from 94.7% to 115%，with intra-day relative standard deviations（intra-RSDs） and inter-RSDs for high and medium concentrations both not more than 15%，as well as the intra-RSDs and inter-RSDs for concentration of quantitative limit not more than 17%．The method is rapid，simple and reproducible，and could meet the requirements for rapid detection of 12 NPS BZDs in urine in the public security field.  
        关键词：direct analysis of real time－tandem mass spectrometry（DART－MS/MS）;urine;NPS of benzodiazepines（DBZDs）   
        45
        |
        10
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706120 false
        发布时间：2023-06-15
      • LIU Xing-sheng,WANG Ai-hua,YU Zhong-shan,LIU Yong-tao,SONG Ge,LIU Yao
        Vol. 42, Issue 6, Pages: 692-698(2023) DOI: 10.19969/j.fxcsxb.23010910
        摘要：A microwave digestion inductively coupled plasma mass spectrometry（ICP－MS） was developed for the determination of metal elements in blood samples．The digestion conditions were optimized，bismuth（Bi） and indium（In） were used as the double internal standard calibration to detect the content of metal elements in postmortem human blood samples and general population control samples．Meanwhile，statistical methods were used to compare the difference and correlation．The results showed that under the digestion conditions of 2 mL hydrogen peroxide，5 mL nitric acid and 190 ℃，the digestion effect was better．There were good linear relationships for nine elements，including magnesium（Mg），chromium（Cr），arsenic（As），strontium（Sr），cadmium（Cd），barium（Ba），mercury（Hg），thallium（Tl） and lead（Pb），with their correlation coefficients（r2） not less than 0.997 7，and the detection limits of 0.000 4－0.049 6 ng/mL．The spiked recoveries ranged from 86.5% to 110%，with the intra-day relative standard deviations（RSDs） and the inter-day RSDs of 0.50%－5.9% and 2.5%－8.5%，respectively，indicating that the recoveries and the precision meet the detection requirements．The Mann－Whitney U test was used to compare the two groups of data since the data of nine metal elements do not conform to Komogorov－Smirnov normality test，and the difference was significant（P < 0.05）．Spearman rank correlation was used to analyze the correlation among metals，and it was found that most metal elements were significantly correlated．A binary logistic regression model was established to investigate the odds ratio（OR） and 95% confidence interval of the sample type and the concentration of metal elements in the blood sample．Mg，Cd and Ba elements were included in the logistic regression model simultaneously．It was found that the results of Mg element were not statistically significant（P > 0.05），Cd and Ba elements were related to the type of blood sample．The detection method and basic data established in this paper could provide important reference and scientific data support for detection and identification of cases related to forensic metal element poisoning.  
        关键词：inductively coupled plasma mass spectrometry（ICP－MS）;statistics;postmortem;blood sample;metallic element   
        57
        |
        13
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706096 false
        发布时间：2023-06-15
      • LI Xiao-fang,ZHOU Wei,YANG Li-wei,WANG Meng-yao,ZHANG Lei,CAI Guo-qiang
        Vol. 42, Issue 6, Pages: 699-706(2023) DOI: 10.19969/j.fxcsxb.23010301
        摘要：A novel method based on ion chromatography was established for the determination of nine chelators in detergent samples．The samples were firstly diluted with deionized water，then purified with IC－RP solid phase extraction columns to eliminate the damage of surfactants in the detergent samples to the chromatographic column，followed by separation on a Dionex IonPacTM AS11－HC anion analysis column with high capacity，using a gradient elution with a high purity of potassium hydroxide（KOH） aqueous solution as the eluent at a flow rate of 1.0 mL/min，which was produced by an automatic generator，and finally detected by Thermo Fisher Intergrion high pressure ion chromatograph with conductivity detector，and quantified using an external standard method．Sodium gluconate（GNa），trisodium methylglycine diacetate（MGDA），nitrous triacetic acid（NTA），hydroxyl ethylidene diphosphonic acid（HEDP），sodium citrate（CANa），sodium pyrophosphate（TSPP），tetrasodium glutamate diacetate（GLDA） and sodium tripolyphosphate（STPP） showed good linear relationships within the range of 1－200 mg/L．Disodium ethylenediamine tetraacetate（EDTA－2Na） showed a good linear relationship in the range of 50－500 mg/L．The correlation coefficients（r） were greater than 0.999．The limit of detection（S/N = 3） and limit of quantitation（S/N = 10） for EDTA－2Na were 12.5 mg/L and 40 mg/L，respectively．The limits of detection and the limits of quantitation for the other eight chelators were in the range of 0.02－0.07 mg/L and 0.06－0.25 mg/L，respectively．The average spiked recoveries at high，medium and low three levels ranged from 92.7% to 106%，with the relative standard deviations（RSDs） of 1.0 %－7.9%，of which all met the detection requirements．Furthermore，twenty-seven detergent samples bought from the market were selected for testing．The results showed that NTA and STPP were not detected in all samples，but EDTA－2Na was found in one dishwasher tablet and one baby bottle cleanser，respectively，and TSPP was detected in three dishwasher powders．GLDA was used as the chelator for most samples of laundry detergents and dishwashing detergents，with the contents of 0.10%－0.25%．The contents of chelators in dishwasher detergents were higher than those in dishwashing detergents and laundry detergents．Chelator played an important role as the main builder in dishwasher detergents．It could not only soften water by complexing calcium，magnesium and heavy metal ions and inhibit the growth of inorganic salt crystals to prevent scale formation，but also disperse the stains in solution and synergize the cleaning effect of surfactants on the stains on tablewares．The total contents of chelators ranged from 3.15% to 25.58% in twelve dishwasher detergents，which were determined in this experiment．Overall，this method was suitable for the determination of nine chelators in detergents for its derivatization-free procedure，simplicity，rapidness，accuracy and sensitivity．Moreover，it could provide a method support for the quality evaluation of detergents.  
        关键词：ion chromatography;chelators;detergents;simultaneous determination   
        37
        |
        12
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706176 false
        发布时间：2023-06-15
      • ZHANG Shan,ZHANG Yan,GAO Yu-meng,HUANG Yao-yao,CAI Hui-shan,WEI Yuan,SU Xiao-dong,ZHOU Qian-yu
        Vol. 42, Issue 6, Pages: 707-714(2023) DOI: 10.19969/j.fxcsxb.22112103
        摘要：A bimetallic co-regulated G-triplex/hemin colorimetric sensing probe for the quantitative analysis of H2O2 was constructed in this paper．Firstly，a G-rich DNA sequence（5′-CTGGGAGGGAGGGA-3′） was bound to hemin，forming a G-triplex/hemin complex with peroxidase-like activity that catalyzes the oxidation of H2O2，causing the reaction substrate to change from colorless to green，which was used as the output module of the sensor．Then by screening the metal ions，it was found that the G-triplex structure could be stabilized in the simultaneous presence of K+ and Sr2+．Under the optimal experimental conditions，the absorbance of the solution showed a good linear relationship with H2O2 in the concentration range of 0.5－4.5 mmol/L，and the limit of detection was 0.07 mmol/L．The method was used for the determination of H2O2 in milk．The spiked recoveries ranged from 92.5% to 103%，with the relative standard deviations of 1.2%－5.4%．With the advantages of short base sequence，low cost and high applicability，the probe provides a new idea for the research of G-triplex functionalized nucleic acid probes.  
        关键词：G-triplex;hemin;K+;Sr2+;colorimetric probe;co-regulated   
        17
        |
        6
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705912 false
        发布时间：2023-06-15
      • YU Qin,WU You-yi,ZHOU Min,CAO Peng
        Vol. 42, Issue 6, Pages: 715-721(2023) DOI: 10.19969/j.fxcsxb.23020602
        摘要：Based on ultrasonic-assisted in-situ formation and solidification of floating deep eutectic solvent（DES），a novel large volume sample stacking capillary electrophoresis with dispersive liquid－liquid microextraction was developed for the determination of four fluoroquinolones（FQs） including gatifloxacin，lomefloxacin，ciprofloxacin and fleroxacin in water samples．In the experiment，methyltrioctyl ammonium bromide and heptanoic acid were chosen as hydrogen bond acceptor（HBA） and hydrogen bond donor（HBD），respectively．Ultrasonication was employed to assist the in-situ formation of deep eutectic solvent，and the synthesized DES was acted as extractant．The experimental conditions affecting the extraction effect were optimized in detail，including the type and volume of DES，parameters of in-situ formation，consumption of salt，vortex time，etc．Experimental results indicated that，the limits of detection（S/N = 3） and the limits of quantitation（S/N = 10） of the method for the four analytes were in the ranges of 0.6－5.5 μg/L and 2.0－18.3 μg/L，respectively，with the enrichment factors of 89－129 times．The spiked recoveries ranged from 75.6% to 110%，with the intra-day and inter-day relative standard deviations（RSDs） of 3.5%－5.9% and 4.5%－7.1%，respectively．The developed method was successfully applied to the detection of FQs in real water samples.  
        关键词：deep eutectic solvent;in-situ formation;dispersive liquid－liquid microextraction;fluoroquinolones;capillary electrophoresis   
        23
        |
        12
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706053 false
        发布时间：2023-06-15
      • LIANG Ming,HU Jun-peng,WU Yu-luan,CHEN Rong-qiao,XIAN Yan-ping,HOU Xiang-chang,DAI Hang,ZHANG Hao-he,LIU Cheng-hao
        Vol. 42, Issue 6, Pages: 722-728(2023) DOI: 10.19969/j.fxcsxb.23030202
        摘要：An ultra high performance liquid chromatography－tandem mass spectrometric method（UPLC－MS/MS） was established for the simultaneous determination of sulfoxaflor and flupyradifurone residues in animal-derived foods．The sulfoxaflor and flupyradifurone were ultrasonic extracted with acetonitrile from the samples，then purified by the dispersion solid-phase extraction method，and finally filtered through a filter membrane and analyzed by UPLC－MS/MS．After separated using an ACQUITY UPLC® HSS T3 column（2.1 mm × 100 mm，1.8 μm） with acetonitrile and 5 mmol/L ammonium acetate-0.1% formic acid solution as the mobile phases，the detection was performed with electrospray ionization in positive ion scanning mode under multi-reaction monitoring mode，and quantified by the external standard calibration．Linear relationships were found within the range of 0.25－20.0 μg/L for sulfoxaflor and flupyradifurone，with their correlation coefficients（r2） of 0.999 3 and 0.999 1，respectively．The limits of detection（LODs） and limits of quantitation（LOQs） were 1.0 μg/kg and 5.0 μg/kg for sulfoxaflor and flupyradifurone，respectively．The average spiked recoveries for the real samples ranged from 90.1% to 113%，with relative standard deviations（RSDs） of 2.5%－7.8%．The method is rapid，simple，accurate，sensitive and reproducible，and it could meet the requirements for determination of sulfoxaflor and flupyradifurone residues in animal-derived foods.  
        关键词：QuEChERS;ultra high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）;animal-derived foods;sulfoxaflor;flupyradifurone   
        29
        |
        12
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705943 false
        发布时间：2023-06-15
      • WANG De-xiang,DUAN Yu,KONG Da-bin,WANG Hong,HU Min-kang,ZHANG Jin-ming,LI Sheng-nan,YANG Wen,DU Hai-jun
        Vol. 42, Issue 6, Pages: 729-735(2023) DOI: 10.19969/j.fxcsxb.22122502
        摘要：A graphene-loaded tin dioxide electrochemical sensor for the electrochemical detection of exogenous plant hormone 4-iodophenoxyacetic acid（4-IPOAA） was fabricated in this paper．The graphene-loaded tin dioxide was constructed by synthesizing coral-like tin dioxide nanoparticles using hydrothermal method and homogeneously immobilizing them on graphene．The results showed that there was a good linearity for 4-IPOAA in the range of 0.5－20 µmol/L and 20－100 µmol/L by square wave voltammetry，and the limit of detection（LOD，S/N = 3） was 9.86 × 10-2 µmol/L．The electrochemical oxidation process of 4-IPOAA was controlled by mixing with the participation of 2 electrons．The prepared sensors showed good reproducibility with relative standard deviations（RSDs） not more than 3.8%．The spiked recoveries were in the range of 91.3%－106% and 91.4%－116% for 4-IPOAA in cabbage and cucumber，with RSDs of 1.1%－5.2% and 3.8%－8.0%，respectively，which indicated that the the sensor has a promising application prospect in the practical analysis of 4-IPOAA.  
        关键词：plant hormones;4-iodophenoxyacetic acid（4-IPOAA）;graphene;tin dioxide;electrochemical detection   
        21
        |
        7
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705898 false
        发布时间：2023-06-15
      • DENG Xiang,HUANG Xiao-mei,DENG Zi-he,Gong An-jie,CHEN Wei
        Vol. 42, Issue 6, Pages: 736-742(2023) DOI: 10.19969/j.fxcsxb.23022802
        摘要：Fluorescence carbon quantum dots（CQDs） were fabricated by hydrothermal method with ginkgo leaf as the raw material，which have an average diameter of 5.5 nm，a maximum excitation wavelength of 335 nm and a maximum emission wavelength of 418 nm．A novel method of CQDs for picric acid（PA） detection was established，based on fluorescence resonance energy transfer（FRET） due to the partial overlap between CQDs fluorescence spectrum and PA absorption spectrum．Under the optimal experimental conditions，there existed a good linear relationship between fluorescence intensity ratio before and after adding PA（I0/I） and PA concentration（c） in the range of 0.2－800 μmol/L，with a correlation coefficient（r） of 0.999 5 and a limit of detection（LOD） of 32 nmol/L．The spiked recoveries for PA in real water samples at 5，40 and 80 μmol/L levels ranged from 98.0% to 104%，with relative standard deviations（RSDs） of 1.0%－3.2%．This method could be used for the sensitive，rapid and efficient detection of PA in real samples.  
        关键词：ginkgo leaf;carbon quantum dots;fluorescent probe;picric acid   
        20
        |
        14
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706238 false
        发布时间：2023-06-15

        Experimental Techniques and Methods

      • XIONG Chen-ru,WU Hao-ping,XU Jing,LUO Si-heng,ZHENG Shu-feng,TANG Li-chao,WANG Ya-jun,XU Yong-bin,LIU Guo-kun
        Vol. 42, Issue 6, Pages: 743-748(2023) DOI: 10.19969/j.fxcsxb.23031203
        摘要：Quality control in the drug production and traceability of commercial drugs are crucial in drug administration．Given that the cumbersome operation and poor anti-interference ability still occur in the common drug analysis methods，realizing efficient and rapid drug analysis remains an unsolved problem．Here，based on the fingerprinting high resolution and trace level high sensitivity of surface-enhanced Raman spectroscopy（SERS），as well as the accurate identification and extraction of weak signals by principal component analysis（PCA），a feasibility study on the product tracing（different manufacturers） and quality control（the same manufacturer） of dextromethorphan hydrobromide cough syrup is well achieved．The classification by support vector machine（SVM） confirms that the identification accuracy for products from different manufacturers is 100% by SERS－PCA．The proposed SERS-based strategy provides an available method for promoting the practical application of “SERS + chemometrics”in the field of drug analysis.  
        关键词：surface-enhanced Raman spectroscopy（SERS）;dextromethorphan hydrobromide;principal component analysis（PCA）;production traceability;quality analysis   
        22
        |
        9
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706152 false
        发布时间：2023-06-15
      • SHAO Lei,WANG Han,LIU Chang-jie,SONG Hai-yun,ZHANG Jian,YANG Chen-guang,CHEN Chi-lai
        Vol. 42, Issue 6, Pages: 749-754(2023) DOI: 10.19969/j.fxcsxb.23011701
        摘要：Underwater mass spectrometry is an important means for in-situ detection of dissolved gas in water．Its quantitative calibration depends on the preparation of different concentrations of dissolved gas，which takes a lot of time．Based on the different physical transport mechanisms，the process of dissolved gas passing through the membrane，pipeline transmission，and analyzer detection was decomposed and analyzed in this paper，then a rapid quantitative method that separates the process of sample passing through the membrane from the mass spectrometry detection process was proposed，and finally an experimental verification was conducted．The results showed that the permeation rate was highly linear with the partial pressure of the sample，with a correlation coefficient（r） of 0.998．Meanwhile，the membrane permeation efficiency could be determined by using a single set of data，and the relative error with the fitting results of multiple sets of data is 3.9%．Furthermore，the pipeline has a significant impact on the permeation rate．The traditional model that does not consider the pressure behind the membrane has a large error，but the pipeline transmission model that considers the pressure behind the membrane could reduce the error by at least 85.4%．The peak heights of the characteristic peaks in the mass spectrum are highly linear with the sample flux，and their correlation coefficients are all greater than 0.999．Based on the above conclusions，the step-by-step quantitative method was verified by using the bubbling method to prepare different concentrations of dissolved gas，and the maximum relative error between the calibration results and the gas chromatograph detection results is 10.9%．Therefore，a new method for rapid calibration of underwater mass spectrometers under time-limited conditions is provided.  
        关键词：underwater mass spectrometer;in situ analysis;membrane injection process;rapid quantitative calibration method   
        26
        |
        9
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705863 false
        发布时间：2023-06-15
      • LIU Cui-mei,SONG Chun-hui,JIA Wei,HUA Zhen-dong,LIAO Qi
        Vol. 42, Issue 6, Pages: 755-761(2023) DOI: 10.19969/j.fxcsxb.23013002
        摘要：A low-field 1H quantitative nuclear magnetic resonance（LF－1H qNMR） spectroscopy was developed for the simultaneous quantification of ketamine and 4 adulterants，i.e. dimethyl sulfone，sulfanilamide，niacinamide，and phenacetin in this paper．Meanwhile，its quantification ability was compared with that of high-field 1H quantitative nuclear magnetic resonance（HF－1H qNMR）．As for LF－1H qNMR，the intra-day relative standard deviations（RSDs），inter-day RSDs，and limit of quantitations（LOQs） for ketamine and 4 adulterants were in the range of 0.50%－2.9%，2.0%－7.4% and 0.3－5 mg/mL，respectively，while for HF－1H qNMR，the intra-day RSDs，inter-day RSDs and LOQs were 0.40%－1.1%，1.5%－3.9% and 0.003－0.05 mg/mL，respectively．Both LF－1H qNMR and HF－1H qNMR were applied to the quantification of 167 seized ketamine samples．The quantitative relative errors of LF－1H qNMR and HF-1H qNMR for ketamine and adulterants were all lower than 15%．The purity ranges of ketamine，dimethyl sulfone，sulfanilamide，niacinamide，and phenacetin determined by LF－1H qNMR were 13.5%－102.6%，1.1%－81.3%，2.6%－83.4%，1.8%－22.7% and 3.4%－43.8%，respectively，while those of ketamine，dimethyl sulfone，sulfanilamide，niacinamide and phenacetin determined by HF－1H qNMR were 13.2%－99.7%，1.0%－78.4%，2.5%－75.9%，1.7%－21.3% and 3.0%－43.5%，respectively．Both LF－1H qNMR and HF-1H qNMR could realize the simultaneous quantitative analysis of ketamine and the adulterants without using reference materials．Although the precision and sensitivity of LF－1H qNMR are slightly lower than those of HF－1H qNMR，its simultaneous quantification ability toward multi-components in complex matrices is exciting．LF－1H qNMR will be more widely used in forensic science laboratories in the future due to its low costs in instrument purchase and daily maintenance.  
        关键词：drug;ketamine;adulterants;quantification;high-field nuclear magnetic resonance spectroscopy;low-field nuclear magnetic resonance spectroscopy   
        18
        |
        7
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705801 false
        发布时间：2023-06-15
      • LIANG Zi-yang,LUO Hui-tai,ZHOU Xi,LIN Xiao-shan,WU Hui-qin,HUANG Fang
        Vol. 42, Issue 6, Pages: 762-767(2023) DOI: 10.19969/j.fxcsxb.23021002
        摘要：A method of QuEChERS/gas chromatography－tandem mass spectrometry（GC－MS/MS） was established for the determination of benvitimod added illegally in cream cosmetics．Cream samples were dispersed with saturated sodium chloride solution and extracted with acetonitrile．After purified with anhydrous magnesium sulfate，PSA and C18，the pretreatment samples were separated on an Agilent VF－17ms capillary column（30 m × 0.25 mm × 0.25 μm），detected by GC－MS/MS in selective reaction monitoring（SRM） mode，and quantified by the matrix-matched calibration．The pretreatment method was optimized by investigating the effects of type and volume of extraction solvent，extraction time，purification composition and dosage on the recovery of benvitimod．Under the optimal conditions，benvitimod showed a good linear relationship in the concentration range of 1－100 μg/L with a correlation coefficient（r2） of 0.999 5．The limit of detection was 0.005 μg/g，and the limit of quantitation was 0.02 μg/g．The spiked recoveries for the target substance ranged from 90.0% to 96.3%，with relative standard deviations（RSDs，n = 6） for repeatability of 1.5%－2.7%，and inter-RSDs and intra-RSDs both less than 10%．The method was applied to the determination of 90 cream cosmetics containing plant extracts，in which one positive sample was found．This method is convenient，accurate and sensitive，and it could provide a technical support for combating illegal addition of cosmetics and ensuring the quality and safety of cosmetics.  
        关键词：gas chromatography－tandem mass spectrometry（GC－MS/MS）;dispersed solid phase extraction;cosmetics;illegal addition;benvitimod   
        24
        |
        8
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38705970 false
        发布时间：2023-06-15
      • CHEN Zi-hao,ZHANG Yong-yi,YANG Jin-yi,ZENG Dao-ping,HE Ying,XU Zhen-lin,WANG Hong,SUN Yuan-ming,SHEN Yu-dong
        Vol. 42, Issue 6, Pages: 768-774(2023) DOI: 10.19969/j.fxcsxb.23022801
        摘要：An indirect competitive enzyme-linked immunosorbent method（icELISA） was developed for the detection of difenoconazole in food and environmental water in this paper，with the coloration from horseradish peroxidase（HRP） catalytically oxidizing tetramethylbenzidine（TMB） as signal output system．Based on the highly specific monoclonal antibody，through the gradual optimization strategy，the optimal immunoassay conditions were determined as follows：the optimal combinations of coating antigen and antibody concentration were 62.5 ng/mL and 0.318 μg/mL，the competitive reaction buffer solution was 0.01 mol/L phosphatic buffer solution containing 0.05% Tween－20（PBST，pH 7.4），the competitive reaction time of the first antibody was 20 min，the diluent of the enzyme-labeled secondary antibody was 0.01 mol/L phosphatic buffer solution（PBS，pH 7.4），and the reaction time of the enzyme-labeled secondary antibody was 30 min．The icELISA for the detection of difenoconazole established under this condition had a linear detection range（IC20－IC80） of 0.49－3.90 ng/mL，a half-inhibition concentration（IC50） of 1.38 ng/mL，and a limit of detection（LOD） of 0.33 ng/mL．The average spiked recoveries for citrus，grape，banana，strawberry field water，lake water and river water samples ranged from 72.3% to 132%，with the relative standard deviations（RSDs） not more than 13%．The cross-reactivities（CRs） against the ten structural and functional analogues were less than 0.2%．The method was accurate and reliable，and it was applicable for rapid screening of difenoconazole in fruit and environmental water samples.  
        关键词：difenoconazole;monoclonal antibody;enzyme-linked immunoassay;fruit;water sample   
        20
        |
        6
        |
        0
        <HTML>
        <L-PDF><Meta-XML>
        <引用本文> <批量引用> 38706209 false
        发布时间：2023-06-15
      0