固相萃取-液质联用法测定刺梨中5种氨基甲酸酯农药

肖洋; 张琼; 叶冲

doi:10.13422/j.cnki.syfjx.2014200091

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固相萃取-液质联用法测定刺梨中5种氨基甲酸酯农药

化学与分析 | 更新时间：2024-01-04

- 固相萃取-液质联用法测定刺梨中5种氨基甲酸酯农药
- Determination of Five Carbamates Pesticide Residues in Rosa Roxburghii Fructus by Solid Phase Extraction and HPLC-MS-MS
- 中国实验方剂学杂志 2014年20卷第20期页码：91-94
- 作者机构：
- 作者简介：
- 基金信息：
  
  国家质检总局科技计划项目（2012QK099）
- DOI：10.13422/j.cnki.syfjx.2014200091
  中图分类号： R284;O657.63
- 纸质出版日期：2014
- 稿件说明：
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肖洋, 张琼, 叶冲. 固相萃取-液质联用法测定刺梨中5种氨基甲酸酯农药[J]. 中国实验方剂学杂志, 2014,20(20):91-94.

XIAO Yang, ZHANG Qiong, YE Chong. Determination of Five Carbamates Pesticide Residues in Rosa Roxburghii Fructus by Solid Phase Extraction and HPLC-MS-MS[J]. Chinese journal of experimental traditional medical formulae, 2014, 20(20): 91-94.
肖洋, 张琼, 叶冲. 固相萃取-液质联用法测定刺梨中5种氨基甲酸酯农药[J]. 中国实验方剂学杂志, 2014,20(20):91-94. DOI： 10.13422/j.cnki.syfjx.2014200091.

XIAO Yang, ZHANG Qiong, YE Chong. Determination of Five Carbamates Pesticide Residues in Rosa Roxburghii Fructus by Solid Phase Extraction and HPLC-MS-MS[J]. Chinese journal of experimental traditional medical formulae, 2014, 20(20): 91-94. DOI： 10.13422/j.cnki.syfjx.2014200091.

摘要

目的：建立刺梨中甲萘威、灭多威、涕灭威、残杀威、克百威等5种氨基甲酸酯类农药残留检测方法。方法：采用高速匀浆制备样品，以乙腈为提取溶剂，提取液浓缩后经氨基固相萃取小柱净化，采用梯度洗脱分离，色谱系统条件为Thermo Hypersil GOLD色谱柱（2.1 mm ×100 mm，1.9 μm），柱温20 ℃，流速300 μL ·min-1，进样量10 μL。在电喷雾正离子模式下，使用三重四级杆质谱仪上以多反应检测模式测定，质谱系统条件为喷雾电压3.0 kV，鞘气压力40 psi，碰撞气压力1.5 mTorr，离子传输管温度350 ℃，蒸发温度250 ℃。结果：5种农药在0.5~100 μg ·L-1线性关系良好，相关系数均>0.999 0，方法检出限为0.2 μg ·kg；低、中、高3个水平的加标平均回收率在77.9%~107.2%，RSD在4.5%~13.2%。结论：该法快速、准确、灵敏，适合刺梨中克百威等5种氨基甲酸酯类农药的残留分析。

Abstract

Objective: To establish one quick method for the determination of five carbamate pesticides including carbaryl

methomyl

aldicarb

suncide and carbofuran in Rosa Roxburghii Fructus by using SPE and HPLC-MS-MS. Method: The sample was cheated by high speed homogenizer

extracted by acetonitrile

cleaned by carbon/NH2 cartridge

separated by gradient elution

the chromatographic condition were column: Thermo Hypersil GOLD columns(2.1 mm ×100 mm

1.9 μm)

temperature 20 ℃

speed 300 μL·min-1

inject 10 μL.Five pesticides were detected with positive-ion electro-spray ionization mass spectrometry in MRM model. The Mass spectrometry condition were spray volage 3.0 kv

sheath gas 40 psi

collision gas pressure 1.5 mTorr

capillary temperature 350 ℃

vaporizer temperature 250 ℃. Result: The calibration curve was liner in the range of 0.5-100 μg ·L-1(r>0.999)

the limits of detection was 0.2 μg·kg; the recoveries were in the range from 77.9% to 107.2% at low

middle and high levels

RSD were 4.5%-13.2%. Conclision: The method is rapid

sensitive and suitable for analyzing carbamate pesticides residues in Rosa Roxburghii Fructus .

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