CAJ | 학술논문

建立了红茶和绿茶中7种硫代氨基甲酸酯类除草剂(禾草敌、克草敌、灭草敌、野麦畏、禾草丹、茵草敌和丁草敌)的高效液相色谱-串联质谱(LC-MS/MS)检测方法.样品制备后,取2.0 g样品,加6 mL水浸润1 h.然后加入2.5 g NaCl,并用20 mL乙腈分两次进行提取,提取液吹氮浓缩后过HLB柱,并用3 mL乙腈洗脱.洗脱液浓缩后用2.0 mL正己烷-丙酮(7∶ 3,V/V)溶解残渣,然后过Envi-Carb固相萃取柱,再用5 mL正己烷-丙酮洗脱,洗脱液浓缩后用乙腈-水(5∶ 5,V/V)定容.采用LC-MS/MS电喷雾电离,多反应监测模式对样品进行分析.以D_3-甲萘威为内标,测定7种硫代氨基甲酸酯除草剂的线性范围为0～200 μg/L,线性相关系数在0.9954～0.9988范围内,检出限在0.093～1.77 μg/L范围内.在添加浓度5～20 μg/kg范围内,7种硫代氨基甲酸酯除草剂的回收率均在77.3%～91.5%,相对标准偏差(RSD)小于15%.本方法被成功用于红茶和绿茶样品中硫代氨基甲酸酯除草剂的测定.
건립료홍다화록다중7충류대안기갑산지류제초제(화초활、극초활、멸초활、야맥외、화초단、인초활화정초활)적고효액상색보-천련질보(LC-MS/MS)검측방법.양품제비후,취2.0 g양품,가6 mL수침윤1 h.연후가입2.5 g NaCl,병용20 mL을정분량차진행제취,제취액취담농축후과HLB주,병용3 mL을정세탈.세탈액농축후용2.0 mL정기완-병동(7∶ 3,V/V)용해잔사,연후과Envi-Carb고상췌취주,재용5 mL정기완-병동세탈,세탈액농축후용을정-수(5∶ 5,V/V)정용.채용LC-MS/MS전분무전리,다반응감측모식대양품진행분석.이D_3-갑내위위내표,측정7충류대안기갑산지제초제적선성범위위0～200 μg/L,선성상관계수재0.9954～0.9988범위내,검출한재0.093～1.77 μg/L범위내.재첨가농도5～20 μg/kg범위내,7충류대안기갑산지제초제적회수솔균재77.3%～91.5%,상대표준편차(RSD)소우15%.본방법피성공용우홍다화록다양품중류대안기갑산지제초제적측정.
A method for the determination of seven kinds of thiocarbamate herbicides, molinate, pebulate, vernolate, triallate, thibencarb, eradicane and butylate in black tea and green tea has been developed. After homogenization, 2.0 g tea sample was soaked with 6 mL water for 1 h. 2.5 g NaCl was then added, and the sample was extracted twice by 20 mL acetonitrile. After concentration, the extract was put through HLB column and eluted by 3 mL acetonitrile. The eluate was then concentrated and dissolved with 2.0 mL hexane-acetone (7∶ 3, V/V) mixture. The preparation was cleaned by Envi-Carb column and eluted with 5 mL hexane-acetone. After concentration, the residue was dissolved by acetonitrile-water (5∶ 5, V/V) solution. Detection was achieved by electrospray ionization(ESI) in positive mode using multiple reaction monitoring. D_3-carbaryl was used as the internal standard, the linear range for the herbicides was 0-200 μg/L and the limit of detection were from 0.093 to 1.77 μg/L, with the correlation coefficients(r) varying from 0.9954 to 0.9988. The recoveries of all thiocarbamate herbicides were from 77.3% to 91.5% at the spiked levels of 5-20 μg/kg. The RSD of each compound was less than 15%. Black tea and green tea samples were successfully analyzed by the proposed method with satisfactory results.