气相色谱-串联质谱法测定黄秋葵中107种农药残留量  

GC-MS/MS Determination of Residual Amounts of 107 Pesticides in Okra

作　　者：林玉婵 陈孟君 杨钦沾 符靖雯 吴燕梅 黄子敬 

机构地区：[1]惠州市农产品质量安全监督检测中心,惠州516008

出　　处：《理化检验（化学分册）》2016年第9期999-1006,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：基金项目:气相色谱-串联质谱测定黄秋葵中多种类农药残留量的方法研究(2014A040401008)

摘　　要：经捣碎的黄秋葵样品(10.0g)中加入乙酸-乙腈(1+99)溶液10mL和氯化钠5g,匀浆提取2min,离心5min;取上清液2.00mL,与无水硫酸镁150mg,N-丙基乙二胺(PSA)25mg和C1825mg涡旋振荡1min作净化处理后离心3min。取其上清液1.00mL,加入100mg·L-1环氧七氯溶液4μL作为内标,按程序升温进样,用Rxi-5Sil MS石英毛细管色谱柱分离。MS/MS分析中采用电子轰击离子源(EI)和多反应监测(MRM)模式。在选定的条件下测定了107种农药的残留量,结果表明:107种农药的线性范围均在0.040~0.80mg·L^(-1)之间,各组分的检出限(3S/N)在0.5~8μg·kg^(-1)之间。在3个浓度水平上作加标回收试验,计算得回收率在65.1%~109%之间,测定值的相对标准偏差(n=6)在2.0%~9.6%之间。The pounded okra sample （10. 0 g） was extracted with 10 mL of a mixture of CH3 COOH-CH3 CN （1＋99） and 5 g of NaC1 by homogenization for 2 min and centrifugation for 5 min. 2.00 mL of the supernatant was taken and mixed with 150 mg of anhydrous MgSO4, and 25 mg each of PSA and C18 for purification by swirling for 1 min and centrifuging for 3 min. 1. 00 mL of the supernatant was taken and 4 μL of 100 mg · L^-1 heptachlorepoxide solution was added to it as internal standard. This mixed solution was used for GC-MS/MS determination of 107 pesticides as residues in okra. Temperature-programmed sample introduction and Rxi-SSil MS quartz capillary chromatographic column were used in GC separation. EI and MRM mode were adopted in MS/MS analysis. As shown by the results, linearities were found for 107 pesticides in the same range of 0. 040-0. 80 mg · L^-1 , with detection limits （3S/N） ranged from 0. 5 to 8 μg · kg^-1. Test for recovery was made by standard addition method at 3 concentration levels, giving values of recovery in the range of 65.1%-109%, and values of RSD （n= 6） found wre in the range of 2.0%-9.6%.

关 键 词：气相色谱-串联质谱法 程序升温进样 农药残留量 黄秋葵 

分 类 号：O657.63[理学—分析化学]