摘要
采用改良的QuEChERS法结合高效液相色谱-串联质谱技术,建立了黄金罗汉果中50种常用农药残留的测定方法。样品采用水-1%(体积分数)乙酸乙腈提取,经900 mg无水MgSO_(4)、450 mg PSA、300 mg C_(18)和50 mg GCB组合吸附剂净化。采用Agilent Poroshell 120 EC-C_(18)色谱柱(150 mm×3.0 mm,2.7μm)分离,0.05%甲酸水溶液(含10 mmol/L甲酸铵)和95%甲醇(含10 mmol/L甲酸铵和0.05%甲酸)为流动相,电喷雾正负离子同时扫描、多反应监测(MRM)模式下检测,基质匹配标准溶液外标法定量。结果显示,50种农药在各自质量浓度范围内线性关系良好,相关系数(r)均大于0.99,定量下限为0.01~0.02 mg/kg。2 LOQ、5 LOQ、20 LOQ、40 LOQ 4个加标水平下的平均回收率为60.7%~115%,95%以上农药的相对标准偏差(RSD)小于15%,符合痕量分析要求。该方法便捷可靠,适用于黄金罗汉果中农药多残留检测。
An improved QuEChERS/high performance liqiud chromatography-tandem mass spec⁃trometry(HPLC-MS/MS)was established for the determination of 50 common pesticide residues in golden siraitia grosvenoriis.After extracted with water-1%(volume fraction)acetic acid acetoni⁃trile,the samples were purified with a combined adsorbent of 900 mg MgSO_(4),450 mg PSA,300 mg C_(18) and 50 mg GCB.Analytes were separated on Agilent Poroshell 120 EC-C_(18) column(150 mm×3.0 mm,2.7μm),using 0.05%formic acid solution(containing 10 mmol/L ammonium formate)and 95%methanol(containing 10 mmol/L ammonium formate and 0.05%formic acid)as mobile phases.Electrospray ionization source was applied in positive and negative ionization(ESI+and ESI-)mode under multiple reaction monitoring(MRM)mode.Meanwhile,the external standard method was employed to obtain the matrix-matched calibration curve for quantitation.Results showed that there existed good linear relationships for 50 pesticides in the respective concentration ranges,with their correlation coefficients(r)larger than 0.99.The limits of quantitation(LOQs)were 0.01-0.02 mg/kg.The average recoveries at four spiked levels of 2 LOQ,5 LOQ,20 LOQ and 40 LOQ ranged from 60.7%to 115%,with relative standard deviations(RSDs)less than 15%for over 95%pesticides,which met with the requirements for trace analysis.This method is convenient and reliable,and it could be applied to the determination of multi-pesticide residues in golden sirai⁃tia grosvenoriis.
作者
李纯
陈俊妃
熊颖
谢思敏
顾利红
LI Chun;CHEN Jun-fei;XIONG Ying;XIE Si-min;GU Li-hong(Guangzhou Institute for Drug Control,NMPA Key Laboratory for Quality Evaluation of Traditional Medicine,Guangzhou 510160,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2022年第12期1793-1799,共7页
Journal of Instrumental Analysis
基金
国家药典委员会项目(2021Z009,2022Z08)。
