CAJ | 학술논문

建立了茶叶中草甘膦( PMG)及其主要代谢物氨甲基膦酸( AMPA)残留检测的高效液相色谱-串联质谱法。样品经水超声,混合相固相萃取小柱净化,加9-芴基甲基三氯甲烷( FMOC-Cl)溶液在硼酸盐缓冲溶液进行衍生化,采用电喷雾离子源、正离子扫描模式和多反应监测模式质谱检测,内标法定量。方法的定量检测低限为0.05 mg/kg,在1.0~20μg/L范围内线性良好,相关系数r2大于0.99,茶叶基质中, PMG和AMPA的3个加标水平下的回收率为65.5%~84.0%,相对标准偏差( RSD, n=6)为3.5%~10.4%。该方法简单、准确性好,能满足日常检测工作的要求。
건립료다협중초감련( PMG)급기주요대사물안갑기련산( AMPA)잔류검측적고효액상색보-천련질보법。양품경수초성,혼합상고상췌취소주정화,가9-물기갑기삼록갑완( FMOC-Cl)용액재붕산염완충용액진행연생화,채용전분무리자원、정리자소묘모식화다반응감측모식질보검측,내표법정량。방법적정량검측저한위0.05 mg/kg,재1.0~20μg/L범위내선성량호,상관계수r2대우0.99,다협기질중, PMG화AMPA적3개가표수평하적회수솔위65.5%~84.0%,상대표준편차( RSD, n=6)위3.5%~10.4%。해방법간단、준학성호,능만족일상검측공작적요구。
A method was developed for the determination of glyphosate ( PMG ) and aminomethylphosphonic acid ( AMPA) in tea using high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS) . The PMG and AMPA were extracted with water under ultrasonication, and cleaned-up using a mixed-mode solid phase extraction ( SPE) cartridge, then PMG and AMPA were derivatized using 9-fluorenylmethoxycarbonyl ( FMOC-Cl) in borate buffer. The detection of target compounds was performed by MS under electrospray ionization source, positive scanning mode and multiple reaction monitoring ( MRM) . The internal standard method was used for the quantitative analysis. The limit of quantification ( LOQ) was 0. 05 mg/kg. Calibration curves of pesticide were linear between 1. 0 μg/L and 20 μg/L, with correlation coefficients of more than 0. 99. The recoveries of PMG and AMPA in tea ranged from 65. 5% to 84. 0%, with relative standard deviations ( RSDs) were between 3. 5% and 10. 4%. The method was simple, accurate and can meet the requirements for daily food determination.