QuEChERS-气相色谱-三重四极杆质谱法测定大蒜中3种农药残留

Determination of 3 kinds of pesticide residues in garlic by QuEChERS-gas chromatography-triple quadrupole mass spectrometry

中文关键词:  敌百虫  霜霉威  氯氟氰菊酯  大蒜  QuEChERS  气相色谱-三重四极杆质谱法

英文关键词:trichlorfon  propamocarb  cyhalothrin  garlic  QuEChERS  gas chromatography-triple quadrupole mass spectrometry

中文摘要:

      目的 建立QuEChERS前处理结合气相色谱-三重四极杆串联质谱联用法测定大蒜中敌百虫、霜霉威和氯氟氰菊酯共3种农药残留的分析方法。方法 将大蒜捣碎, 用乙腈-醋酸(99:1, V:V)、无水硫酸镁、醋酸钠和陶瓷均质子提取, 经无水硫酸镁和乙二胺-N-丙基甲硅烷(ethylenediamine-N-propylsilane, PSA)净化, 用DB-1701P毛细管柱进行分离, 在电子轰击离子源(electron impact source, EI)和多反应离子监测(multiple reaction monitoring, MRM)模式测定, 基质标准曲线校正, 内标法定量。结果 3种待测物在5.00~ 5000.00 ng/mL范围内呈良好线性, 相关系数(r2)均大于0.99, 定量限(limits of quantification, LOQ)均为 0.01 mg/kg, 在3个添加水平(0.01、0.10、1.00 mg/kg)下, 加标回收率范围为73.23%~110.00%, 相对标准偏差(relative standard deviation, RSD)为1.33%~8.14%。结论 该方法简单、灵敏、准确, 适用于大蒜中敌百虫、霜霉威和氯氟氰菊酯的快速筛查和定量测定。

英文摘要:

      Objective To establish a method for the determination of trichlorfon, propamocarb and cypermethrin residues in garlic by QuEChERS pretreatment combined with gas chromatography-triple quadrupole tandem mass spectrometry. Methods Garlic was mashed, extracted with acetonitrile-acetic acid (99:1, V:V), anhydrous magnesium sulfate, sodium acetate and ceramic homo-protons, purified by anhydrous magnesium sulfate and ethylenediamine-N-propylsilyl, and separated by using a DB-1701P capillary column. The results were measured in an electron bombardment source and multi-reaction ion monitoring mode, corrected by the matrix standard curve, and quantified by the internal standard method. Results The linearity was good over the range of 5.00?5000.00 ng/mL, correlation coefficients (r2) were greater than 0.99, and limits of quantification were 0.01 mg/kg. The recoveries were in the range of 73.23%?110.00% at the 3 addition levels (0.01, 0.10, and 1.00 mg/kg). The relative standard deviations were 1.33%?8.14%. Conclusion This method is simple, sensitive and accurate, and is suitable for rapid screening and quantitative determination of trichlorfon, propamocarb and cypermethrin in garlic.