QuEChERS-GC-MS/MS测定化橘红65种农药残留  

Determination of 65 Pesticide Residues in Citri Grandis Exocarpium by QuEChERS-GC-MS/MS

作　　者：熊颖[1] 李纯[1] 侯惠婵[1] 顾利红[1] 栗建明[1] 王艳慧 XIONG Ying;LI Chun;HOU Hui-chan;GU Li-hong;LI Jian-ming;WANG Yan-hui(Guangzhou Institute for Drug Control/Key Laboratory for Quality Evaluation of Traditional Chinese Medicine(Traditional Chinese Patent Medicine),National Medical Products Administration,Guangzhou 510160,China;Guangzhou Xiangxue Pharmaceutical Co.,Ltd.,Guangzhou 510663,China)

机构地区：[1]广州市药品检验所/国家药品监督管理局中成药质量评价重点实验室,广东广州510160 [2]广州市香雪制药股份有限公司,广东广州510663

出　　处：《中国现代中药》2021年第6期1043-1050,共8页Modern Chinese Medicine

基　　金：国家重点研发计划中医药现代化研究重点专项(2018YFC1706700)。

摘　　要：目的:建立气相色谱-串联质谱法(GC-MS/MS)检测化橘红中65种农药残留。方法:样品经乙腈匀浆提取,固相分散萃取(QuEChERS)管净化,采用DB-17MS毛细管柱(30 m×0.25 mm,0.25μm),载气为氦气,进样口温度为250℃,进样量为1μL,程序升温(0~1 min,60℃;以30℃·min^(-1)升至120℃;以10℃·min_(-1)升至160℃;以2℃·min-1升至230℃;以15℃·min-1升至300℃,保持6 min;升至310℃,保持5 min),传输接口温度为280℃;质谱离子源温度为280℃,电子轰击离子源(EI);轰击能量为70 eV;碰撞气为氮气,多反应监测(MRM)模式,空白基质配对照品法测定。结果:65种农药线性关系良好,r均大于0.995,添加水平0.01 mg·kg^(-1)时平均回收率为70.63%~127.65%,RSD为0.97%~8.85%;添加水平0.02 mg·kg^(-1)时平均回收率为67.05%~130.26%,RSD为0.52%~5.27%,检出限为0.002~0.010 mg·kg^(-1)。结论:该方法可判断化橘红是否有农药残留,为化橘红农药残留限度标准制定提供参考。Objective:To establish a gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the determination of 65 pesticide residues in Citri Grandis Exocarpium.Methods:Citri Grandis Exocarpium sample was extracted with acetonitrile by homogenization and purified by dispersive solid-phase extraction(QuEChERS).The GC conditions are as follows:DB-17MS capillary column(30 m×0.25 mm,0.25μm),carrier gas of helium,injection port temperature of 250℃,injection volume of 1μL,temperature programming(0-1 min,60℃;increasing to 120℃at 30℃·min^(-1);rising to 160℃at 10℃·min^(-1);elevating to 230℃ at 2℃·min-1;growing to 300℃at 15℃·min-1 and keeping at 300℃for 6 min;increasing to 310℃and maintaining at 310℃for 5 min),interface temperature of 280℃.MS conditions are as below:ion source temperature of 280℃,electron impact ionization(EI)with energy of 70 eV,collision gas of nitrogen,multiple reaction monitoring(MRM).The blank matrix-matched reference substance method was adopted for the measurement.Results:The calibration curves of 65 pesticide residues showed good linearity with correlation coefficients(r s)>0.995.At the spiked level of 0.01 mg·kg^(-1),the average recoveries were 70.63%-127.65%,with relative standard deviations(RSDs)of 0.97%-8.85%.At the spiked level of 0.02 mg·kg^(-1),the average recoveries were 67.05%-130.26%,with RSDs of 0.52%-5.27%.Limit of Quantitation(LOQ)was in the range of 0.002-0.010 mg·kg^(-1).Conclusion:The method can be used to determine whether Citri Grandis Exocarpium contains pesticide residues.The result can serve as a reference for the formulation of pesticide residue limit standard for Citri Grandis Exocarpium.

关 键 词：化橘红 农药残留 固相分散萃取 气相色谱-串联质谱法 

分 类 号：R284[医药卫生—中药学]