最新刊期
      卷 37 ， 期 8 ， 2018
      • Vol. 37, Issue 8, Pages: 871-878(2018)
        摘要：A rapid and sensitive method was developed for the analysis of 6 polybrominated biphenyl ethers(PBDEs) at trace levels in environmental water samples by gas chromatography-tandem mass spectrometry(GC-MS/MS) with a synthesized zeolite imidazolate framework-8(ZIF-8) as solid phase microextraction coating.The experimental conditions were optimized with single factor tests，and the optimal conditions were as follows：extraction time：50 min，extraction temperature：50 ℃，pH value：70，desorption temperature：280 ℃，desorption time：5 min，and without salt addition.Under the optimized conditions，the calibration curves for 6 PBDEs were linear in the range of 1-1 000 ng/L with limits of detection and limits of quantitation of 008-229 ng/L and 023-732 ng/L,respectively.The intra day and inter day RSDs were in the range of 43%-65% and 69%-93%，respectively.This method was successfully applied in the analysis of PBDEs in 4 environmental water samples(tap water，spring water，pond water and landfill waste water) with recoveries of 816%-109%.  
        关键词：zeolite imidazolate framework-8;polybrominated biphenyl ethers(PBDEs);solid phase microextraction(SPME);gas chromatography-tandem mass spectrometry(GC-MS/MS)   
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      • Vol. 37, Issue 8, Pages: 879-886(2018)
        摘要：A method for the determination of 187 kinds of pesticides in dried persimmon by liquid chromatography-tandem mass spectrometry（LC-MS/MS） was established.The samples were extracted with acetonitrile containing 1% acetic acid，then purified with anhydrous magnesium sulfate，anhydrous sodium acetate，anhydrous sodium sulfate，N propyl ethylenediamine（PSA） and C18.The separation of targeted compounds was performed on a ZORBAX Eclipse Plus-C18 column by gradient elution using 95% acetonitrile aqueous solution（organic phase） and water（aqueous phase） as mobile phases，both contained 0005 mol/L ammonium formate and 001% formic acid.The compounds were detected by LC-MS/MS with positive electrospray ion source（ESI+） under dynamic multiple reaction monitoring（DMRM） mode.The matrix-matched external standard method was used for the quantitation.The callibration curves for 187 pesticides were linear in the range of 1-100 μg/kg with correlation coefficients（r2） more than 099.The limits of detection（S/N≥3） and quantitation（S/N≥10） for the analytes were 1 μg/kg and 10 μg/kg，respectively.The recoveries were in the range of 702%-118% with relative standard deviations（RSDs，n=6） of 20%-20%.The method is suitable for the high throughput detection on pesticide multi residues in dried persimmon with its advantages of accuracy，sensitivity and rapidness.  
        关键词：liquid chromatography-tandem mass spectrometry（LC-MS/MS）;positive electrospray ion source;dried persimmon;pesticide multi residue   
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      • Vol. 37, Issue 8, Pages: 887-893(2018)
        摘要：An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS／MS) method was developed for the determination of 10 pyrethroid pesticide residues in animal foods.The samples were extracted with glacial acetic acid-acetonitrile（1∶99，by volume），and most of the oil impurities were removed by cryogenic freezing，and then further purified with Z-Sep+ and C18.The separation of target compounds was performed with ACQUITY HSS T3 column using 01% formic acid aqueous solution containing 5 mmol/L ammonium acetate and methanol as mobile phases，and the detection of pesticides was carried out in electrospray ionization under multiple reaction monitoring mode.Results showed that the calibration curves for 10 pyrethroids were linear in the range of 25-100 μg/L with their correlation coefficients all larger than 0997.The limits of detection were in the range of 09-24 μg/kg and the limits of quantitation were 30-80 μg/kg.The spiked recoveries for 10 pyrethroid pesticides at three levels of 10，50 and 100 μg/kg were in the range of 703%- 120% with relative standard deviations（RSDs）of 12%-112%.With simple pretreatment，high sensitivity and good accuracy，the method completed detection on the targets within 10 min，and could meet the requirements for rapid detection of 10 pyrethroid pesticide residues in animal foods.  
        关键词：pyrethroid;animal food;zirconium dioxide;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS／MS);matrix effect   
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      • Vol. 37, Issue 8, Pages: 894-899(2018)
        摘要：Two interface devices for online supercritical fluid chromatography（SFC）were developed for the determination of solubility of anthracene in supercritical carbon dioxide and its dissolving equilibrium according to the static and dynamic operating modes.The static interface was consisted of two high pressure valves，and the dynamic interface was composed of one high pressure valve and one gear pump.The gear pump built into the dynamic interface maintained a constant flow of supercritical fluid carbon dioxide solution from the solubility vessel through the interface sample injection valve in a return flow circuit.The solubility of anthracene in supercritical carbon dioxide was measured by static method，the impacts of temperature and pressure on solubility were investigated，and the obtained solubility data were correlatedly calculated according to the density based on model of Méndez-Santiago Teja（MST）.A series of progressively more concentrated anthracene/carbon dioxide solutions were separately prepared by increasing the pressure in controlled steps.Solubility of anthracene was measured at 40，50 and 60 ℃ in the pressure range of 100-275 MPa using 25 MPa steps.The experimental results demonstrated that good stability and reproducibility for the self-developed equipment were acquired with RSD value range of 04%-24% and experimental accuracy of 950%-977%.All sets of experimental solubility data were correlated according to the density based MST model，the calculated average absolute relative deviation（AARD）values were 323 and 1468，respectively.The developed interface devices could become a bridge for the combination of conventional analytical equipments such as FT-IR/UV/mass spectrometry with supercritical fluid technique in applications of online monitoring pharmaceutical compound synthesis and analysis，process analysis technique（PAT）.  
        关键词：online supercritical fluid chromatography;interface;solubility;carbon dioxide   
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      • Vol. 37, Issue 8, Pages: 900-905(2018)
        摘要：A method based on high performance liquid chromatography（HPLC） with online monolithic column solid phase extraction was developed for the determination of diflubenzuron and hexa flumuron in fruits. The polymer（poly（2 ethylhexyl methacrylate co ethylene dimethacrylate）） monolithic column（10 mm×46 mm，id.） was prepared by using 2 ethylhexyl methacrylate（EHMA） as monomer and ethylene dimethacrylate（EDMA） as crosslinker，which exhibited a porous structure with a specific surface area of 16401 m2·g-1. Using polymer monolithic column as online solid phase extraction sorbent，the extracted fruit sample solution was loaded into the monolithic column using 5 mmol·L-1 NH4OAc at a flow rate of 01 mL·min-1. The adsorbed analytes were transferred from monolithic column to the analytical column using acetonitrile-water（65∶35，by volume） as mobile phase at a flow rate of 10 mL·min-1. Under the optimized conditions，there was a good linearty for the method in the range of 01-500 mg·L-1（r≥0998）. The limits of detection and quantitation for diflubenzuron and hexaflumuron were 0007 2 mg·kg-1 and 0009 mg·kg-1，and 0024 mg·kg-1 and 0030 mg·kg-1，respectively. The recoveries at three spiked levels of 003，03 and 15 mg·kg-1 were in the range of 895%-102% with intra day and inter day relative standard deviations not more than 68%.  
        关键词：benzoylurea insecticides;polymer based monolithic column;online solid phase extraction;high performance liquid chromatography（HPLC）;fruit   
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      • Vol. 37, Issue 8, Pages: 906-912(2018)
        摘要：The understanding of size distribution and chemical composition of aerosol particles in human exhaled breath could provide helpful information for disease diagnosis，environmental exposure assessment，etc.In this study，the feasibility for simultaneously acquiring the size distribution and chemical composition of exhaled breath particles（EBPs） of human by single particle aerosol mass spectrometry（SPAMS） was preliminarily investigated.The EBPs were dried with a Nafion tubing，then directly analyzed by SPAMS.The number concentration of EBPs for a healthy adult is about 227-1 043 pcs/L，and the limit of detection（LOD） for obtaining a representative size distribution profile is 2 500 pieces，which means approximately 10 L of breath sample is required for the analysis.The exhaled particles sizes dominantly ranged from 200 nm to 1 000 nm，and the peak was observed at 460 nm.For the exhaled particles，the size distribution and chemical profiles reflect the information involving both exogenous and endogenous particles.Compared with that for particles in ambient air，the size distribution profile for exhaled particles contained higher abundance of relative particle numbers（RPNs） in the ranges of 200-300 nm and 440-660 nm，which were lower than or comparable with the RPNs in the ranges of 320-420 nm and 680-2 000 nm.Regarding the chemical composition，it was speculated that the higher presence of CxHyO+z（x=1~3，y=1~7，z=1~3），PO-3，CN- and CNO- in the exhaled particles（680-2 000 nm） might result from the endogenous phosphatidylglycerol and protein，whereas C-3、C-4、C+、C+3、C3H+and C+4in the range of 200-300 nm concern with the carbon of exogenous particles in the inhaled air.  
        关键词：human exhaled breath;aerosol particle;single particle mass spectrometry;size distribution;chemical composition   
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      • Vol. 37, Issue 8, Pages: 913-918(2018)
        摘要：A method of stirring bar sorptive extraction（SBSE） based on mussel-bioinspired chemistry coating and high performance liquid chromatography with fluorescence detector（HPLC/FLD） was developed for the simultaneous determination of aflatoxin B1，B2，G1 and G2（AFB1，AFB2，AFG1 and AFG2） in edible oil.The sample was extracted by SBSE with dopamine-graphene oxide complex as solid phase extraction material prepared by mussel-bioinspired chemistry.The target compounds were separated on a Kromasil C18 column using methanol-acetonitrile-water aqueous solution（3∶3∶5 by volume，adjust pH 35 with 10%phosphoric acid） as mobile phases，and detected with a fluorescence detector.The calibration curves for AFB1，AFB2，AFG1 and AFG2 were linear in the concentration range of 0200-100 μg/L，with their correlation coefficients（r2） not less than 0998 9.The spkied recoveries for 4 aflatoxins（AFs） in edible oil samples ranged from 815% to 969%，with intra day relative standard deviations（RSDs） of 17%-34% and inter day RSDs of 19%-35%.The limits of detection（LODs） were in the range of 0025-0050 μg/L.The proposed method is efficient，sensitive and reliable，and is suitable for the determination of AFB1，AFB2，AFG1 and AFG2 in edible oil.  
        关键词：mussel-bioinspired chemistry;dopamine-graphene oxide complex;stirring bar sorptive extraction（SBSE）;high performance liquid chromatography with fluorescence detector（HPLC/FLD）;edible oil;aflatoxin（AF）   
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      • Vol. 37, Issue 8, Pages: 919-924(2018)
        摘要：A method was developed for the determination of trace Pb2+in surface water by microwave plasma atomic emission spectrometry with ion imprinted polymer solid phase extraction（IISPE/MP-AES）.The ion imprinted polymer microspheres（IIPMs） were synthesized via Pickering emulsion polymerization with Pb2+as template ions.Results showed that IIPMs exhibited a porous structure with an average particle diameter of 266 μm，which resulted in their high selectivity and monolayer adsorption toward Pb2+.The solid phase extraction process was conducted with IIPMs as sorbent and 5%nitric acid as elution solvent.Factors affecting preconcentration such as pH value，cycle number，concentration and adding amount of Pb2+were investigated.Under the optimized experimental conditions，the limits of detection（LODs） of the method were 026 μg/L，and the spiked recoveries were in the range of 924%-988%with relative standard deviations（RSDs） not more than 41%.The combination of IIPMs-SPE and MP-AES was successfully applied in the determination of trace lead in surface water.  
        关键词：ion imprinting solid phase extraction（IISPE）;Pickering emulsion polymerization;lead;MP-AES;surface water   
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      • Vol. 37, Issue 8, Pages: 925-929(2018)
        摘要：An analytical method was developed for the simultaneous determination of trifluoroacetate and trifluoromethanesulfonate by reversed phase liquid chromatography with indirect ultraviolet detection using pyridinium ionic liquids as mobile phase additives.The chromatographic behaviors of the two anions on the C18 column were studied and compared with four types of reagents including pyridinium ionic liquid，imidazolium ionic liquid，4 aminophenol hydrochloride and tetrabutylammonium chloride as mobile phase additives.Effects of concentrations of pyridinium ionic liquids，organic solvents and detection wavelength on separation and detection of the anions were investigated.The role of ionic liquids，retention rules and relevant mechanisms were discussed.Pyridinium ionic liquids acted as ion pair reagent and ultraviolet absorption reagent in separation and detection of the anions.The separation of the anions was performed on a C18 reserved phase column using methanol-03 mmol/L N hexylpyridine bromide（10∶90，by volume) as mobile phase at a column temperature of 30 ℃，a flow rate of 10 mL/min and a detection wavelength of 250 nm.Under these conditions，two anions were completely separated in 12 min.The detection limits were 009 mg/L and 018 mg/L，respectively.The method was applied in the determination of trifluoroacetate and trifluoromethanesulfonate in ionic liquid samples with spiked recoveries of 960%-101%.The method is simple，accurate and practical.  
        关键词：ionic liquid;liquid chromatography;indirect ultraviolet detection;trifluoroacetate;trifluoromethanesulfonate   
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      • Vol. 37, Issue 8, Pages: 930-934(2018)
        摘要：A method was developed for the determination of migration of 5 ethanolamine compounds in food contact materials by liquid chromatography-tandem mass spectrometry（LC-MS/MS）.Samples were soaked with five food simulants（water，4% acetic acid，10% ethanol，50% ethanol，95% ethanol）.4% acetic acid soaking solution was dried out with nitrogen，and then rehydrated with water.Other soaking solutions were injected directly after filtration with membrane.The separation of target compounds was performed with an amino column BEH Amide（50 mm×21 mm，17 μm），using acetonitrile-5 mmol/L ammonium acetate as mobile phase by gradient elution.The detection on the analyte was performed with positive electrospray ionization source under multiple reaction monitoring（MRM） mode，and the quantitation was carried out by external standard method.Under the optimized conditions，the calibration curves were linear in the range of 10-7500 μg/L，with correlation coefficients larger than 0997.The limits of detection（LODs，S/N=3） and quantitation（LOQs，S/N=10） were in the ranges of 03-50 μg/kg and 10-150 μg/kg，respectively.The average recoveries for 5 ethanolamine compounds at the spiked levels of 10-7500 μg/kg were in the range of 902%-118%，with relative standard deviations of 05%-88%.The method is sensitive and accurate，and could meet the requirements for correlative determination.  
        关键词：food contact material;ethanolamine compounds;liquid chromatography-tandem mass spectrometry（LC-MS/MS）;migration   
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      • Vol. 37, Issue 8, Pages: 935-939(2018)
        摘要：A fast and sensitive reversed high performance liquid chromatographic（HPLC） method was developed for the simultaneous detection of three ginsenosides,ie.Rg1,Re and Rb1 in Chinese herbal residues.Effects of solvent,temperature,solvent matrix ratio and time on extraction efficiency were investigated.The sample was ultrasonically extracted with 10 times liquid of 70% methanol at 40 ℃ for 05 h.Chromatographic separation was performed on a Zorbax SB-C18（46 mm×150 mm,5 μm） column by gradient elution using water-acetonitrile as mobile phase at a flow rate of 10 mL/min.The injection volume was 20 μL,the column temperature was 20 ℃ and the detection wavelength was 203 nm.External calibration of peak area versus concentration was used for the quantitation.There were excellent linearities for ginsenosides Rg1，Re and Rb1 in the ranges of 1874-25761,3748-46854 and 388-9693 mg/L,respectively，with their correlation coefficients all above 0999.The limits of quantitation（LOQ,S/N=10） for Rg1,Re and Rb1 were 1769,1394 and 114 mg/L,respectively.The average recoveries at three spiked levels were in the range of 891%-107%,with relative standard deviations（RSD,n=3） of 06%-41%.The method was applied in the detection of ginsenosides Rg1，Re and Rg1 in Chinese herbal samples with simplicity,rapidness and high sensitivity.  
        关键词：ginsenosides;high performance liquid chromatography（HPLC）;Chinese herbal residues   
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      • Vol. 37, Issue 8, Pages: 940-944(2018)
        摘要：An analytical method based on gas chromatography-triple quadrupole mass spectrometry with accelerated solvent extraction（ASE/GC-MS/MS） was established for the simultaneous determination of 24 polycyclic aromatic hydrocarbons（PAHs） in textiles.PAHs in the samples were extracted by ASE with acetone,and evaporated to dryness with a rotary evaporator.The separation was performed on a DB-35 capillary column by temperature programming.The identification was performed by GC-MS/MS in multiple reaction monitoring（MRM） mode，and the quantitation was carried out by the external standard method.The calibration curves for 24 PAHs showed good linearities in the certain concentration with correlation coefficients（r2） larger than 0994.The limits of detection（LODs） and quantitation（LOQs） for PAHs in textiles were in the ranges of 0000 3-003 mg/kg and 0001-010 mg/kg,respectively.The average recoveries were in the range of 803%-103% with relative standard deviations（RSDs,n=6） of 13%-92%.The method is suitable for the simultaneous determination of 24 PAHs in textiles with high sensitivity,accuracy and reliability.  
        关键词：gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）;accelerated solvent extraction（ASE）;textile;polycyclic aromatic hydrocarbon（PAHs）   
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      • Vol. 37, Issue 8, Pages: 945-949(2018)
        摘要：A method was established for the determination of chiral difenoconazole in dragon fruit by solid phase extraction coupled with high performance liquid chromatography.The dragon fruit samples were extracted with acetonitrile，and purified with carbon black/amino solid phase extraction column.Effects of different chiral columns，mobile phase compositions，flow rates and injection volumes on chiral separation were investigated.The optimized chromatographic conditions were as follows：the chromatographic column：IF-3 chiral column，mobile phase：n hexane-ethanol（92∶8 by volume），injection volume：60 μL，flow rate：10 mL/min.Under the optimized conditions，the four difenoconazole enantiomers were basically achieved baseline separation，and the analysis time was less than 35 min.There existed a good linearity for each enantiomer in the range of 010-10 mg/L，with a detection limit of 0025 mg/L.The average recoveries for the chiral difenoconazole in dragon fruit at two spiked levels of 04 mg/kg and 28 mg/kg were in the ranges of 837%-993% and 864%-916%，with their RSDs of 13%-72% and 14%-31%，respectively.The developed method is rapid，accurate and sensitive，and is applicable for the determination of chiral difenoconazole residues in dragon fruit，etc.  
        关键词：solid phase extraction(SPE);high performance liquid chromatography（HPLC）;dragon fruit;difenoconazole enantiomers;chiral pesticides   
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      • Vol. 37, Issue 8, Pages: 950-954(2018)
        摘要：A method for the determination of desmopressin in urine by liquid chromatography-tandem mass spectrometry was established.The sample was purified by Waters C18 solid phase extraction，and separated on a Phenomenx Onyx C18 chromatographic column.The analysis on the target compound was performed by MS in positive ion ionization under multiple reaction monitoring（MRM） mode.Total of eight volunteers were invited to reserve their urine samples within 3 d after each took a single-dose of desmopressin.The samples were detected by the established method and the metabolic curves for the analyte were drawn out.Results showed that the limits of detection of the method were 02 μg/L.There were linearities for desmopressin in the range of 05-20 μg/L with correlation coefficients（r2） larger than 0997.The recoveries at three spiked levels of low，medium and high concentrations were all higher than 59%，with the intra day and inter day precisions all less than 10%，and the matrix effects within 20%.The peak concentrations of desmopressin in eight volunteers occurred within 70-150 min after taking the drug，and the highest concentrations were in the range of 02-24 μg/L.The longest detection window period could last for about 13 h.This method is unique for the detection of desmopressin in urine，and fully meets the requirements of the World Anti doping Agency for 2 μg/L concentration of the drug by reducing the experiment time and the experimental cost.This method was used to analyze the positive urine after taking the drug，and the elimination of desmopressin in the human body was also investigated.  
        关键词：doping control;liquid chromatography-tandem mass spectrometry（LC-MS/MS）;desmopressin;human urine;elimination   
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      • Vol. 37, Issue 8, Pages: 955-961(2018)
        摘要：The volatile components of four different types of animal oils，eg.chicken oil，tallow，goat oil and lard oil，were determined.In perspective of the volatile flavor substances of animal oils，the possibilities of distinguishing and classifying different types of animal oils were explored.A gas chromatography-mass spectrometry with thermal desorption(TD/GC-MS) was performed for the determination of the quasi-determinacy and relative contents of volatile components in four animal oils，while principal component analysis，cluster analysis and discriminant analysis were applied in the analysis of the principal components of volatiles in the oils based on SPSS 220 statistical software.According to the flavor threshold value and characteristics of volatile compounds and their relative contents，the principal component analysis(PCA) was used after the variables and index gains and losses.A total of 19 main flavor substances were screened out from the 53 volatile components in the four animal oils，and their relative contents were reduced to obtain three principal components.Based on this，three canonical discriminant function models for animal oils were established by using the results of principal component analysis in turn for cluster analysis and discriminant analysis.The accuracies for discriminating the volatile components of chicken oil，tallow，goat oil and lard oil by the training models reached to 100%.  
        关键词：animal oil;thermal desorption/gas chromatography-mass spectrometry(TD/GC-MS);volatile components;principal component analysis;cluster analysis;discriminant analysis   
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      • Vol. 37, Issue 8, Pages: 962-966(2018)
        摘要：A method of anion exchange high performance liquid chromatography was developed for the determination of five nucleotides，including cytidine monophosphate(CMP)，adenosine monophosphate(AMP)，uridine monophosphate(UMP)，guanosine monophosphate(GMP) and inosine monophosphate(IMP).The samples were extracted with water，then precipitated protein with precipitants.The determination of analytes was performed by HPLC on a Sax column using methanol-KH2PO4（10 mmol/L，pH 45） as mobile phase by gradient elution.The detection wavelength was set at 254 nm，and the external standard method was used for quantitation.Result showed that there were good linearities for five nucleotides in the concentration range of 0200-200 mg/L，with their correlation coefficients（r） of 0999 8-1000 0.The spiked recoveries were in the range of 955%-108% with RSDs of 10%-32%.With the advantages of good separation，wide linear range，good stability and accuracy，the method solved the matrix interference problem in sample detection based on GB 541340-2016 52，and enriched the chromatographic conditions for GB 541340-2016.  
        关键词：high performance liquid chromatography（HPLC）;strong anion exchange（SAX）;nucleotides;matrix interference;infants and young children;food and milk products   
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      • Vol. 37, Issue 8, Pages: 967-971(2018)
        摘要：A smartphone digital colorimetric method was proposed for the rapid detection of sulfonamides based on the aptamer/AuNPs complexation structure.Aptamers were bound on the surfaces of AuNPs by the electrostatic interaction which changed the charge density of the nanoparticles surfaces and the complexation of AuNPs with aptamers，preventing the nanoparticles from aggregating in a high salt solution.The solution kept a stable red.In the presence of sulfonamides，the weaker binding between aptamers and the AuNPs was broken，and sulfonamides bound up with aptamers.The specific and stronger binding between sulfonamides and the aptamers led to the separation of the aptamers from the surfaces of the nanoparticles.The nanoparticles began to aggregate，which could result in a color changed from red to purple-blue.In order to achieve a precise，quantitative，fast and convenient detection，a smartphone was arranged to capture the digital images.The complementary wavelength of images was analyzed by a smartphone App，and the concentration of sulfadimethoxine（SDM） in the range of 0-5 μg/mL could be determined by analyzing the correlation between SDM concentration and the complementary wavelength.The method showed high sensitivity，and the detection limit was 013 μg/mL.  
        关键词：nanoparticles aggregation;digital colorimetric method;aptamers;antibiotics detection;smartphone App   
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      • Vol. 37, Issue 8, Pages: 972-976(2018)
        摘要：A sensitive liquid chromatography-tandem mass spectrometric（LC-MS/MS) method was developed for the determination of pyridostigmine bromide in feed.The sample was extracted with acetonitrile or methanol，then concentrated to dryness under nitrogen，finally dissolved in water.The extract was purified with n hexane and solid phase extraction（SPE) column，then separated on a C18（150 mm×30 mm，3 μm) column by gradient elution using acetonitrile-5 mmol/L ammonium formate solution as mobile phase at a flow rate of 03 mL/min and a column temperature of 40 ℃.The qualitative analysis was performed with electrospray ionization in positive mode（ESI+) under multiple reaction monitoring（MRM) mode，and the quantitation was carried out by the isotope internal standard method.Results indicated that the calibration curves for pyridostigmine bromide in different feed matrixes showed good linear relationships in the concentration range of 1-100 μg/L with their correlation coefficients all above 0999.The limits of detection and quantitation were 10 μg/kg and 20 μg/kg，respectively.The recoveries ranged from 961% to 108% with relative standard deviations（RSDs) of 28%-83%.The method is sensitive and accurate，and is suitable for the determination of pyridostigmine bromide in compound feed，concentrated feed，additive premix and concentrate supplement.  
        关键词：liquid chromatography-tandem mass spectrometry（LC-MS/MS);feed;pyridostigmine bromide   
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      • Vol. 37, Issue 8, Pages: 977-980(2018)
        摘要：A method was developed for the determination of semicarbazide（SEM） by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The degradation of azodicarbazide（ADA） to SEM under heat treatment was also studied.The method was optimized by using 2 nitrobenzaldehyde as derivative agent，at a derivative temperature of 37 ℃ and an extraction pH value of 70.The calibration curve was linear in the range of 05-100 μg·L-1 with a correlation coefficient（r） of 0999 and a detection limit of 04 μg·L-1The spiked recoveries at three spiked levels of 10，20 and 40 μg·L-1 were in the range of 996%-120%with relative standard deviations less than 7.6%.Results showed that ADA was degraded into SEM under heat treatment，and it was degraded completely at high temperature.Meanwhile，the formation rate of SEM increased with the increase of temperature，and it reached the maximum value of 0094% at 200 ℃.Nevertheless，the formation rate decreased with the decomposition of SEM when the temperature was exorbitant（>200 ℃）.Besides，it also decreased when the baking time lasted too long（>30 min）.  
        关键词：high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）;azodicarbazide;semicarbazide;heat treatment   
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      • Vol. 37, Issue 8, Pages: 981-988(2018)
        摘要：Macrolide drug residues have become an attention focus in field of the food safety inspection.In this paper，the background and current status of research on veterinary macrolides are summarized，the distribution of macrolides and their metabolites in livestock and poultry are described，and the pre processing and detection methods for macrolide residues in foods are reviewed.Fortheremore，the development tendency for analysis of macrolide drugs and their metabolites residues is also look forward to.  
        关键词：meat food;macrolide drug residues;metabolite;pre processing;detection method   
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