Research On Detection Of 13 Kinds Of Carbamates In The Textile And Edifenphos In Grain

Due to the frequent occurrence of security incidents in textiles and food in recent years,people pay more and more attention on the safety of textiles and food.At the same time,the security problem of textile has also had a great impact on China's foreign trade.After the implementation of the "Positive List System" in Japan,the problem of pesticide residues in grain in China has also become an important factor restricting foreign trade.In view of the previous reasons,A method for the determination of 13 carbamates in textiles by high performance liquid chromatography(HPLC)tandem high resolution mass spectrometry,a method for the study of Edifenphos in grain by HPLC –MS/MS and by GC were established in this paper.Part I:The high performance liquid chromatography-trandem high resolution mass spectrometry(HPLC-HRMS)was applied to determine the carbamates residues(including Aminocarb?Carbaryl?Pirimicarb?Methiocarb?Indoxacarb?Aldicarb?aldicarb sulfone?aldicarb sulfoxide?Carbofuran?3-hydroxy carbofuran?Isoprocarb?Metolcarb?Propoxur)in the textile.The pretreatment method was evaluated based on Qu ECh ERS method to improve the recovery of every analyst.The analytes were extracted using Acetonitrile as extraction solvent.The separation of carbamates compounds was performed on a Agilent SBC18 column using acetonitrile-20 mmol/L ammonium acetate solution containing0.1 % formic acid and 0.1 % formic acid aqueous solution as mobile phase in a gradient elution mode.The results showed that the limit of quantification for the analytes for 13 carbamates compounds were between 0.50 ?g/L and 5.0 ?g/L.And the recoveries of the analytes at three spiked levels were between 79.89 % and 94.20 % with the relative standard deviations of 4.78~11.95 %.The present method is accurate,reliable and can beapplied to the determination of carbamates residues in textile.Part II:This method was established for the study of Edifenphos in grain(Rice,millet,brown rice,corn,flour)by the high performance liquid chromatography-trandem high resolution mass spectrometry(HPLC –MS/MS).The analyst was extracted by acetonitrile-water solution(9+1),and then purified by Pro Elut AFT-3 solid phase extraction(SPE)cartridge.The separation of Edifenphos compounds was performed on a XBridge C18 column using acetonitrile solution and 0.1 % formic acid aqueous solution as mobile phase in a gradient elution mode.The results showed that the limit of quantification for the analytes was 0.30 ?g/L.And the recoveries of the analytes at three spiked levels were between 75.0% and 108.2 % with the relative standard deviations lower than 9.48 % in the range of 1.0 to 100.0 ?g·L-1.The present method use less time and material,the target was detected at 3.08 min and can be applied to the determination of Edifenphos residues ingrain.Part III:This method was established for the study of Edifenphos in grain by gas chromatography(GC).The analyst was extracted by acetonitrile-water solution(9+1),and then purified by Pro Elut AFT-3 cartridge.The separation of Edifenphos compounds was performed on a DB-5(30m*0.25mm*0.25?m)column.The results showed that the limit of quantification for the analytes was 0.05mg/kg.And the recoveries of the analytes at three spiked levels were between 65.4 and 116.0% with the relative standard deviations lower than 16.86 % in the range of 1.0 to 100.0 ?g·L-1.The present method was easy and accurate,the target was detected at7.8 min and can be applied to the determination of Edifenphos residues ingrain.