最新刊期
      卷 42 ， 期 7 ， 2023

        Scientific Papers

      • QIU Tian,BAO Shan,JIANG Wei-long,LU Yi-fu
        Vol. 42, Issue 7, Pages: 775-783(2023) DOI: 10.19969/j.fxcsxb.23031003
        摘要：A gas chromatography－tandem mass spectrometric（GC－MS/MS） method was developed for the simultaneous analysis of 43 persistent organochlorine pollutants（POCPs），including 18 polychlorinated biphenyls（PCBs） and 25 organochlorine pesticides（OCPs） in human serum，based on solvent extraction coupled with solid-phase extraction cartridge cleanup．Human serum samples were thawed and brought to room temperature before pretreatment．An aliquot of 250 µL serum sample was transferred into a 12 mL glass tube．Protein was precipitated using methanol and lipid was removed by acidification to release target analytes．A liquid－liquid extraction was performed using hexane and methyl tert-butyl ether in turn．The extract from both solvent was combined and concentrated．The sample was further purified using silica gel solid-phase extraction cartridges，then concentrated to near-dryness under gentle stream of nitrogen and reconstituted with toluene．Subsequently，the chromatographic separation was performed on a TG-5SilMS（30 m × 0.25 mm × 0.25 µm） column．The target analytes were monitored under multiple reaction monitoring（MRM） mode，and quantified by internal standard method．The results showed that there were good linear relations for the 18 PCBs and 25 OCPs in the ranges of 0.008－1 µg/L and 0.08－10 µg/L，with the detection limits and the quantitation limits of 0.005－0.1 µg/L and 0.02－0.3 µg/L，respectively．The matrix effect was in the range of 74.9%－126%．The spiked recoveries ranged from 71.6% to 129%，with intra-day relative standard deviations（RSDs） and inter-day RSDs of 1.0%－11% and 1.3%－18%，respectively．To evaluate method accuracy，standard reference material purchased from the US National Institute of Standards and Technology was used．The relative deviations of tested results were lower than 30% compared to certified values．The developed method was applied to the determination of 173 serum samples collected from general population．A total of 28 POCPs were detected，of which p，p′-DDE and PCB 153 both had a detection frequency over 50%，and the median concentration of p，p′-DDE was found to be 0.46 µg/L，making it the primary POCPs in the serum samples of this particular population．This analytical method is suitable for the detection on 43 POCPs in human serum samples as it could effectively control the matrix effect and improve the analytical sensitivity.  
        关键词：gas chromatography－tandem mass spectrometry;persistent organochlorine pollutants;liquid－liquid extraction;solid-phase extraction;human serum   
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        发布时间：2023-07-12
      • SONG Jin-peng,LIANG Kun,ZHANG Chi,MEI Xiu-ming,JIANG Peng-fei,YUAN Rui
        Vol. 42, Issue 7, Pages: 784-793(2023) DOI: 10.19969/j.fxcsxb.23030501
        摘要：In view of the need for rapid and non-destructive detection of common bunt，a visible-near infrared spectroscopy combined with deep learning algorithms was proposed to construct a classification model for identifying common bunt of wheat kernels in this paper．The spectral data were preprocessed by multiple scattering correction（MSC） and standard normal variate（SNV） algorithms to eliminate noise．Meanwhile，feature wavelength extraction was performed on the preprocessed spectra using the competitive adaptive reweighted sampling（CARS） and random frog（RF） algorithms．The results indicated that the feature extraction algorithms effectively removed redundant information，resulting in a reduction of 93.7% to 94.2% in the number of spectral bands. This significantly reduced the model’s computational cost and prevented overfitting．The achieved results demonstrated the effectiveness of the MSC + CARS + VGG16 model with an accuracy of 96.39% for the training set and 91.67% for the test set，providing satisfactory classification outcomes．The final VGG16 deep learning model successfully categorized wheat kernels into three classes：healthy，light suscept，and heavy suscept．Compared to traditional machine learning models，the VGG16 model demonstrates a superior capability in extracting spectral features，and could more accurately distinguish healthy wheats and light suscept wheats．Results showed that visible-near infrared spectroscopy combined with deep learning could realize the effective classification on the wheat kernels with different degrees of common bunt，providing a novel approach for the rapid and non-destructive detection on common bunt wheat kernels.  
        关键词：visible－near infrared spectroscopy;deep learning;common bunt;wheat   
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        发布时间：2023-07-12
      • GUO Zong-ning,YE Ling-yun,ZHANG Xiao-lin,ZHANG Ni,HUANG Xue-lin,JIAO Zhe
        Vol. 42, Issue 7, Pages: 794-800(2023) DOI: 10.19969/j.fxcsxb.23022402
        摘要：Development of an affordable，simple and on-site method for the assessment of SARS－CoV－2 exposure is critical to guarantee the safety of public environments．In this paper，a visual discrimination method for SARS－CoV－2 polluted aerosol was developed based on portable polymerase chain reaction（PCR） instrument，water-soluble AIE luminogens（AIEgens） and air sampler．The positive plasmid sample was firstly amplified by PCR，then visualized by DNA-binding AIEgens 1，1，2，2-tetrakis［4-（2-bromo-ethoxy） phenyl］ ethene（TTAPE） with a label-free approach．The lighted-up emission could be distinctly identified with naked eye under a UV lamp or a portable smartphone．The results showed that positive plasmid could be visually detected，which confirmed the specificity of the proposed method．The portable system was applied to the on-site screening of SARS－CoV－2 in real aerosol samples，with the results all negative.  
        关键词：SARS－CoV－2;AIEgens;visual;on-site;aerosol   
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        发布时间：2023-07-12
      • OUYANG Li,JIANG Shun,HU Li-li,WANG Hui,DENG Nan,YANG Yun
        Vol. 42, Issue 7, Pages: 801-807(2023) DOI: 10.19969/j.fxcsxb.23031902
        摘要：A QuEChERS/ultra-high performance liquid chromatography－tandem mass spectrometric（UPLC－MS/MS） method was established for the simultaneous determination of 15 coumarins and 10 benzophenones in sunscreen cosmetics．The samples including cream，foundation，isolation and spray were extracted with acetonitrile，and purified with a combined adsorbent of 50 mg C18 and 150 mg anhydrous MgSO4．The chromatographic separation for the analytes was achieved on a Zorbax SB－C18（RRHD） column（2.1 mm × 150 mm，1.8 µm）. Gradient elution was performed using 0.1% formic acid solution（containing 5 mmol/L ammonium acetate） and acetonitrile．Then the analytes were determined with electrospray ionization in positive ion mode under multiple reaction monitoring（MRM），and quantified by external standard method，while the analytes in foundation and spray samples were quantified by matrix-matched external standard method．The experimental results indicated that good linearities were observed for 25 kinds of analytes in the respective concentration ranges，with their correlation coefficients（r） larger than 0.995．The limits of detection（LODs） and limits of quantitation（LOQs） for cream and isolation samples were in the ranges of 0.005－0.450 μg/g and 0.010－0.750 μg/g，while the LODs and LOQs for foundation and spray samples were 0.005－0.500 μg/g and 0.010－1.000 μg/g，respectively．Mean recoveries for the analytes at three spiked levels ranged from 80.8% to 113%，with relative standard deviations（RSDs） of 0.20%－6.8%．Moreover，the analytes in the sample solutions were stable within 48 hours．The proposed method is simple，sensitive and accurate，and it could be applied to the simultaneous determination of coumarin and benzophenone compounds in cosmetics.  
        关键词：QuEChERS;ultra-high performance liquid chromatography－tandem mass spectrometry;sunscreen cosmetics;coumarin;benzophenone   
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        发布时间：2023-07-12
      • YANG Yan-mei,LI Jin-dong,QIN Shu
        Vol. 42, Issue 7, Pages: 808-816(2023) DOI: 10.19969/j.fxcsxb.23030703
        摘要：An ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with QuEChERS was established for the simultaneous determination of 60 pesticides and 24 antibiotics in soil．The samples were extracted with Na2EDTA－Mcllvaine buffer solution（pH 7.20） and acetonitrile solution containing 5.0%（by volume） formic acid，then purified with octadecyl silane（C18） and primary secondary amine（PSA）．Analytes were separated on an ACQUITY UPLC BEH C18 column（2.1 mm × 100 mm，1.7 µm），then detected under multiple reaction monitoring（MRM） mode，and quantified by matrix-matched standard solutions and external standard method．Results showed that there existed good linear relationships for 84 compounds in their respective concentration ranges，with correlation coefficients（r2） not less than 0.990．The limits of quantitation（LOQs） of 81 compounds were 0.01 mg/kg except for LOQs of thiophanate-methyl，doxycycline and chlortetracycline were 0.1 mg/kg．The recoveries ranged from 60.9% to 118%，with relative standard deviations（RSDs，n = 5） of 0.38%－22%．This method is simple，sensitive and accurate，and it could be applied to the determination of pesticides and antibiotics in soil.  
        关键词：QuEChERS;ultra performance liquid chromatography－tandem mass spectrometry （UPLC－MS/MS）;soil;pesticides;antibiotics   
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        发布时间：2023-07-12
      • ZHANG Hao,GAO Shu-hui
        Vol. 42, Issue 7, Pages: 817-824(2023) DOI: 10.19969/j.fxcsxb.23040403
        摘要：Vehicle’s paint chips are one of the common physical evidences at the scene of criminal cases and traffic accidents. Identification and recognition of such physical evidences have been an important part of the research of public security technicians as they might contain some important information about the vehicles involved．Traditional instrumental analysis methods are cumbersome and cannot meet the demand for rapid nondestructive testing of physical evidence at the scene．Based on the advantages of nondestructive imaging and simple operation of spectral detection，a hyperspectral imaging technology combined with deep residual shrinkage network was explored to identify on-site car paint evidence，in order to improve detection efficiency and optimize detection means．The hyperspectral images of 54 car paint samples from 18 different car models were collected，and the images were fused with 10 × 10 pixels to form a reflection spectrum of 19 740 pixels．Combined with the characteristics of hyperspectral data，a targeted one-dimensional deep residual shrinkage network（1D-DRSN） recognition model was established in this paper．The results showed that 1D－DRSN model has 99.5% and 98.6% accuracy for the training and test sets，with the loss function values decreasing to 0.093 and 0.106，respectively．1D-DRSN was significantly better than 1D convolutional neural network（1D-CNN） model and three traditional machine learning methods，including support vector machine（SVM），random forest（RF） and logistic regression（LR）．The white car paint samples from different brands or models are distinguished by deep mining of hyperspectral data．This study was applied to solving the practical challenges，and it will be a powerful complement to the existing techniques and methods in the detection and classification of vehicle’s paint fragments from the scene.  
        关键词：hyperspectral imaging technique;deep residual shrinkage network;machine learning;car paint evidence from the scene;intelligent identification   
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        发布时间：2023-07-12
      • WANG Tao,ZHANG Hong,ZHOU Han-lin,LIN Jie,TONG Ping,BEN Yu-jie,WANG Yao-qiang,HAN Yong-he,ZHANG Yong,LI Jia-bing
        Vol. 42, Issue 7, Pages: 825-832(2023) DOI: 10.19969/j.fxcsxb.23032803
        摘要：An effective analytical method was established for the determination of 12 organophosphate esters（OPEs） in soil by solid phase extraction coupled with high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） in this paper．After freeze-drying and sieving，the soil samples were ultrasonically extracted with acetone－hexane（1∶1，by volume），then purified with a CNWBOND Florisil SPE cartridge，and finally analyzed by HPLC－MS/MS．The internal standard method was used for quantification．There were good linear relationships for 12 OPEs in the concentration range of 0.1－100 μg/L，with correlation coefficients（r2） greater than 0.999 and detection limits of 0.004－0.162 ng/g．The average recoveries at low，medium and high three spiked levels ranged from 67.0% to 128%，with relative standard deviations of 1.5%－9.9%．12 OPEs were detected simultaneously in 20 soil samples by the method established．All target compounds were detected with a total content of OPEs ranging from 5.36 to 55.2 ng/g（dry weight），the mean value of 23.7 ng/g（dry weight） and the median value of 25.0 ng/g（dry weight）．This method is suitable for the determination of OPEs in soil samples with sensitive and reliable results.  
        关键词：organophosphate esters;soil;solid phase extraction;high performance liquid chromatography－tandem mass spectrometry   
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        发布时间：2023-07-12
      • WANG Xu-feng,WANG Qiang,ZHANG Ying-xia,HUANG Ke
        Vol. 42, Issue 7, Pages: 833-840(2023) DOI: 10.19969/j.fxcsxb.23040604
        摘要：A multi-residue analytical method was established for the simultaneous determination of ten tranquilizers and their metabolites in aquatic products by pass-through solid phase extraction（SPE） in combination with ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）．Samples were extracted with 1% ammonium hydroxide－ethyl acetate，followed by one-step cleanup based on KNORTH m-PFC SPE cartridge．The purified extractions were blew to dryness under nitrogen gas．The dried residues were dissolved with 0.5 mL acetonitrile and then injected into UPLC－MS/MS．The chromatographic separation of ten target analytes were conducted on a JADE－PAK KP－C18 column（100 mm × 2.1 mm，1.7 μm） by gradient elution，utilizing 0.1% formic acid－acetonitrile and 0.1% formic acid solution as mobile phases．The targeted analytes were analyzed with positive electrospray ionization under multiple reaction monitoring（MRM） mode，confirmed using ion ratio and retention time，and quantitated by internal standard method．Excellent linearities for ten target analytes were obtained in the corresponding mass concentration ranges，with correlation coefficients（r2） larger than 0.999．The limits of detection and the limits of quantitation for aquatic product samples were in the range of 0.1－0.15 μg/kg and 0.3－0.5 μg/kg，respectively．The average recoveries for four negative aquatic product matrixes at three spiked levels ranged from 82.6% to 117%，with relative standard deviations（RSDs，n = 6） of 1.5%－9.3%．The proposed method is sensitive and versatile，and it can be applied to the multi-residue analysis of ten tranquilizers and their metabolites in various aquatic product matrixes.  
        关键词：tranquilizers;metabolite;pass-through solid phase extraction;ultra-performance liquid chromatography－mass spectrometry;aquatic product   
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        发布时间：2023-07-12
      • ZHAO Shan-shan,YANG Xiao-ting,ZHAO Hong-yang,LIU Hao,LIU Nan,SUN Li-rong,LU Xing-an,ZHAO Yan
        Vol. 42, Issue 7, Pages: 841-848(2023) DOI: 10.19969/j.fxcsxb.23031702
        摘要：It is necessary to develop new meat stable isotope reference materials to improve the accuracy of stable isotope technology for meat origin tracing applications as few meat isotope reference materials are available from the certified sources．In this paper，two new defatted powdered mutton reference materials（RMs） GSB 11－3959－2022 and GSB 11－3960－2022 with different δ13C and δ15N values were developed，and their homogeneity，the short- and long-term stability were studied．A joint evaluation was performed by elemental analyzer－isotope ratio mass spectrometry（EA－IRMS） in 7 national laboratories．All reported data were tested by Grubbs criterion，Dixon criterion and Cochrane criterion，while the outliers were removed and the property values and uncertainties were obtained．The valued δ13C and δ15N for the GSB 11－3960－2022 were （-18.27 ± 0.26）‰ and （3.25 ± 0.16）‰，respectively．The valued δ13C and δ15N for the GSB 11－3959－2022 were （-19.72 ± 0.23）‰ and （5.29 ± 0.14）‰，respectively．The two mutton isotope reference materials developed in this paper provide a reference for the determination of carbon and nitrogen stable isotope ratios in meat.  
        关键词：defatted powdered mutton;reference materials;elemental analyzer－isotope ratio mass spectrometry;homogeneity;stability   
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        发布时间：2023-07-12
      • CAO Li,LI Ju-ying,YU Jia,DOU Ye-zhi,ZHANG Yue-qing,XU Jing,HE Jian,WU Wen-zhu,KONG De-yang
        Vol. 42, Issue 7, Pages: 849-855(2023) DOI: 10.19969/j.fxcsxb.23020702
        摘要：A liquid chromatography－tandem mass spectrometry（LC－MS/MS） was established for the simultaneous determination of thiencarbazone-methyl and its metabolites including BYH18636-carboxylic acid（M01），BYH18636-sulfonamide-carboxylic acid（M03），BYH18636-sulfonamide（M15） in water，soil and sediments．Water samples were firstly acidated by formic acid，then extracted with HLB solid phase extraction（SPE） cartridge，while the soil and sediments samples were firstly extracted with acidated acetonitrile and cleaned up with primary secondary amine（PSA） cartridge，then detected by LC－MS/MS．The separation was carried out on an Agilent Poroshell 120EC－C18（2.1 mm × 75 mm，2.7 μm） column by gradient elution with acetonitrile and water as the mobile phases．The detection was carried out with electrospray ion source in negative ion mode under multi-reaction monitoring（MRM） mode．External standard method was applied to obtain the matrix-matched calibration curve for quantification．Results showed that there were good linear relationships for thiencarbazone-methyl and its metabolites in the range of 0.001－0.1 mg/L，with their correlation coefficients（r2） more than 0.995．The average recoveries for water samples at three spiked levels of 0.1，1 and 10 µg/L ranged from 75.5% to 104%，with relative standard deviations（RSDs，n = 5） of 1.4%－8.6%，while the recoveries for soil and sediment samples at three spiked levels of 0.5，5 and 50 µg/kg ranged from 75.4% to 105%，with RSDs of 1.5%－9.7%．The quantification limit of four analytes was 0.1 µg/L in water，while 0.5 µg/kg in soil and sediments．With high sensitivity，accuracy and good repeatability，this method is suitable for the simultaneous determination of thiencarbazone-methyl and its metabolites in water，soil and sediments.  
        关键词：thiencarbazone-methyl;metabolites;liquid chromatography－mass spectrometry;solid phase extraction   
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        发布时间：2023-07-12
      • LIU Zheng-hong,LIU Shi-min,ZHU Rong,MING De-wang,ZHOU Qin,CAO Shu-rui
        Vol. 42, Issue 7, Pages: 856-862(2023) DOI: 10.19969/j.fxcsxb.23030302
        摘要：A novel type of nano-carbon composite，magnetic reduced graphene oxide/metal-organic frameworks（MrGO/ZIF－67） was synthesized by combining Fe3O4 nanoparticles with metal-organic framework（ZIF－67） and reduced graphene oxide（rGO），which was employed for the efficient adsorption of methamphetamine（MAMP）．Based on this，a novel ultra-high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with magnetic solid phase extraction（MSPE） was established for the rapid determination of MAMP in hair．Scanning electronic microscopy（SEM），transmission electronic microscopy（TEM），Fourier transform infrared spectroscopy（FT－IR） and vibrating sample magnetometer（VSM） were adopted for the comprehensive characterization of MrGO/ZIF－67．The results showed that Fe3O4 magnetic nanoparticles were successfully attached to the surface of carbon composite．MrGO/ZIF－67 possessed a three-dimensional porous structure，multifunctional groups，and sufficient magnetic force for rapid separation by external magnets．A variety of experimental parameters affecting the sample pretreatment effects were evaluated and optimized．The effect of the solution pH value（2.0 to 12.0） was firstly screened by the one-variable-at-a-time（OVAT） analysis，and single factor experiment showed that the solution pH of 11.0 was the most favorable for the adsorption of MAMP．The influences of magnetic nanomaterials amount（1－5 mg），extraction time（10－90 min） and initial concentration of MAMP（100－500 μg/L） on the adsorption performance of MAMP were further investigated via a three level Box-Behnken design and response surface methodology（RSM）．According to the model recommendations，the optimal extraction conditions were as follows：MrGO/ZIF dosage：4 mg，extraction time：20 min，initial concentration of MAMP：110 μg/L．The results showed that there was a good linear relationship for MAMP in the range of 1－200 μg/L，with a correlation coefficient（r2） of 0.999 9，a limit of detection（LOD） of 0.188 μg/L，and a limit of quantitation（LOQ） of 0.572 μg/L．It was found that MrGO/ZIF－67 material had good adsorption capacity，fast adsorption kinetics and easy separation．The spiked recoveries for the actual hair samples at three levels of 1.0，5.0 and 9.6 μg/L ranged from 80.2% to 94.4%，with intra-day and inter-day relative standard deviations（RSDs，n = 3） of 1.6％－2.7% and 6.0%－8.2%，respectively，indicating that the method had good linearity，high sensitivity，good accuracy and precision．The synthesized magnetic nano-carbon composite MrGO/ZIF－67 and the developed UPLC－MS/MS method could be used to adsorb and detect the content of MAMP in actual hair samples.  
        关键词：MrGO/ZIF－67 composite;magnetic nano carbon materials;methamphetamine;hair   
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        发布时间：2023-07-12

        Experimental Techniques and Methods

      • MENG Xun,LI Xiao-xuan,LI Peng-hui,YIN Zheng,WU Sheng-li
        Vol. 42, Issue 7, Pages: 863-869(2023) DOI: 10.19969/j.fxcsxb.23030101
        摘要：Microplastics insoluble particles of chemical injections of different manufacturers，batches and varieties were detected and analyzed by microscopic infrared spectrometer and confocal laser Raman spectrometer．The results showed that the average concentrations of plastic particles with particle size of lower than 30 μm，30－100 μm and larger than 100 μm were 18.6，8.65 and 0.85 pieces/L，respectively．Meanwhile，the materials of plastic particles include polypropylene（PP），polyethylene（PE），polystyrene（PS） and polyester（PET），and the average concentrations of the above four plastic particles in the injections were 21.05，5.85，0.3 and 0.4 pieces/L，respectively．This is the first time to propose the detection and analysis of plastic particles in insoluble particles of chemical injections in this paper．Although the content of plastic particles is far below the standard value stipulated in the Chinese Pharmacopoeia，it suggests the potential risk of chemical injections.  
        关键词：microplastics;microscopic infrared;microraman;chemical injection;particle size analysis   
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        发布时间：2023-07-12
      • YANG Meng,LI Ying,LI Jian,LI Wei-han,LIU Yan
        Vol. 42, Issue 7, Pages: 870-875(2023) DOI: 10.19969/j.fxcsxb.23030103
        摘要：Strict control and accurate measurement of impurity content in high-temperature alloys are particularly important as the trace impurity elements in high-temperature alloys may have a certain impact on the performance of high-temperature alloys．A triple quadrupole inductively coupled plasma tandem mass spectrometry（ICP－MS/MS） was applied to the direct determination of 15 impurity elements in Fe－Ni based superalloys．The sample was firstly digested with a mixture of nitric acid，hydrochloric acid and hydrofluoric acid，then directly determined on the machine after constant volume，without the need for extraction and separation，greatly improving the efficiency of pre-treatment analysis．In the helium collision mode，the testing and analysis of impurity elements with less interference in high-purity iron-nickel based high-temperature alloys were achieved．As 95Mo16O+ in the superalloy samples with high molybdenum content will cause strong mass spectrum interference to the determination of 111Cd，the single quadrupole mass spectrometer test is limited．Based on this，the superior reaction cell technology of ICP－MS/MS was used in this paper to set the mass-to-charge ratio（m/z） of the primary mass filter（Q1） to 111，and add O2 to the collision reaction pool，so that 95Mo16O+ reacted with O2 to generate 95Mo16O16O+，and then setting the m/z of the secondary mass filter（Q2） to 111，so that 111Cd was passed and detected，thus avoiding the overlapping interference of mass spectra，and stable testing of Cd content was achieved．This study was validated using the iron nickel based high-temperature alloy standard material（GBW01620） as a sample．The results showed that the linear correlation coefficients for each element were greater than 0.999，the detection limits of the method were 0.001－1.24 mg/kg，and the relative standard deviations were not larger than 3.5%．The test values for the 15 elements were all within the uncertainty range of the determined values．This method provides an idea or reference for accurate testing and analysis of high-purity alloy samples.  
        关键词：ICP－MS/MS;Fe－Ni based superalloy;O2 in situ mass mode;He collision mode;impurity element;111Cd   
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        发布时间：2023-07-12
      • HU Wei-qi,LIU Qiu-fen,DING Ya,SHEN Wen-bin
        Vol. 42, Issue 7, Pages: 876-881(2023) DOI: 10.19969/j.fxcsxb.23022706
        摘要：A quantitative nuclear magnetic resonance（1H qNMR） method was developed for the determination of the absolute content of nirmatrelvir API．Based on the conformationally stable conditions of nemativir in solution，the proton signals at δ4.96（1H，dd），δ4.67（1H，dd） and δ6.22（1H，t），δ5.84（1H，d） were selected as the quantitative peaks for nirmatrelvir and lamivudine respectively in DMSO-D6 and D2O（5∶1，by volume） solvents on BRUKER AV－500 NMR instrument．The qNMR method exhibited a high specificity，and an linear fitting equation Y = 0.456 4X - 0.000 5（r2 = 0.999 9） was obtained in the range of 0.5∶1.0－1.2∶1.0 for the molar ratio of sample to internal standard，and the results showed good durability，reproducibility，recovery and 48-hour stability．The content of nirmatrelvir was determined to be 99.23%（RSD = 0.24%） by qNMR．The 1H qNMR method is simple，non-destructive，accurate and rapid，which is suitable for determination on the absolute content of nirmatrelvir API.  
        关键词：nirmatrelvir;lamivudine;quantitative NMR;content determination   
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        发布时间：2023-07-12
      • TIAN Liang-liang,QU Xin,FANG Chang-ling,HUANG Dong-mei,HUANG Xuan-yun,TANG Yun-yu,SHI Yong-fu
        Vol. 42, Issue 7, Pages: 882-887(2023) DOI: 10.19969/j.fxcsxb.23032301
        摘要：A gas chromatography－mass spectrometry（GC－MS） with dispersive solid-phase extraction was developed for the analysis of earthy-musty odorants，including geosmin（GSM） and 2-methylisoborneol（2-MIB） in tap water．n-hexane liquid－liquid extraction（LLE） combined with silica dispersion solid-phase（DSP） was used to isolate the analytes in tap water．The pretreatment conditions including the volume of extractant，time of DSP and eluent ratio were optimized．The optimal experimental conditions were as follows：the samples were extracted with 15 mL n-hexane，then the targets in extract solution were absorbed with 0.5 g silica for 7 min，and finally，1 mL n-hexane/ethyl acetate（1∶1，by volume） was used to elute the compounds．The chromatographic conditions for detection of GSM and 2-MIB were optimized，then the supernatant was determined by GC－MS in selected ion monitoring（SIM） mode，and quantified by the internal standard method．The results showed that there were good linearities for GSM and 2-MIB in the range of 0.5－500 ng/mL，with correlation coefficients（r2） greater than 0.999．The limits of detection（LODs） for GSM and 2-MIB were 0.8 ng/L and 0.4 ng/L，respectively，while the limits of quantitation（LOQs） for GSM and 2-MIB were 2.5 ng/L and 1.5 ng/L，respectively．The average recoveries for GSM and 2-MIB in tap water，at five spiked levels of 4，8，20，80，400 ng/L ranged from 72.7% to 114%，with relative standard deviations（RSDs） of 1.1%－7.8%．The method is simple in operation and accurate in quantification，and it is suitable for the determination of GSM and 2-MIB in tap water.  
        关键词：geosmin（GSM）;2-methylisoborneol（2-MIB）;hexane;silica;gas chromatography－mass spectrometry（GC－MS）;tap water   
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        发布时间：2023-07-12
      • LI Zhi-xuan,ZHAN She-xia,LI Zhi-tu,ZHANG Chang-li,ZHAO Qian-ning
        Vol. 42, Issue 7, Pages: 888-892(2023) DOI: 10.19969/j.fxcsxb.23030102
        摘要：An ultrahigh performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） was established for the determination of three cyanotoxins，i.e. saxitoxin（STX），cylindrospermopsin（CYN） and anatoxins（AnTX） in water．The optimal chromatographic and mass spectrometric conditions were obtained through investigating the influence of chromatographic column，mobile phase and gradient elution program on the separation．The results showed that the three target analytes were effectively separated by gradient elution procedure with formic acid water（0.1%） and acetonitrile as the mobile phases．The limits of detection（LODs） of the method for STX，CYN，AnTX were 0.018，0.009 and 0.013 μg/L，while the correlation coefficients（r） were all higher than 0.999．The recoveries at a spiked level of 0.50 μg/L ranged from 102% to 104%，with the relative standard deviations of 1.7%－5.2%．This method is sensitive，accurate，simple and rapid，and it is suitable for the simultaneous detection of three cyanotoxins with low concentration in water.  
        关键词：ultrahigh performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）;anatoxin;saxitoxin;cylindrospermopsin;water   
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        发布时间：2023-07-12
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