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[液相色谱-串联质谱法测定农产品中烯虫酯的分析方法]

[Analytical method of hydramethylnon in agricultural products by LC-MS/MS].

作者信息

Takahashi Kunihiko, Matsumoto Ryuji, Nemoto Satoru, Matsuda Rieko

机构信息

Saitama Institute of Public Health, Sakura-ku, Saitama-shi, Saitama, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2011;52(1):47-50. doi: 10.3358/shokueishi.52.47.

Abstract

A simple determination method of hydramethylnon in agricultural products by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The sample was homogenized with phosphoric acid and extracted with acetone. An aliquot of crude extract was re-extracted with hexane and sat. NaCl solution. In the case of tea leaf, solidification processing using ammonium chloride and phosphoric acid was performed before re-extraction with hexane. Clean-up was performed using a silica-gel mini column (500 mg). The LC separation was performed on a C18 column using methanol-water (8 : 2) containing 10 mM ammonium acetate as the mobile phase and MS detection with positive ion electrospray ionization. The calibration curve was linear between 0.002-0.2 µg/mL of hydramethylnon. Recoveries (n=5) of hydromethylnon from 10 kinds of agricultural products fortified at 0.01 µg/g (0.05 µg/g for pineapple) were 82-110%, and their relative standard deviations were 2-12%.

摘要

建立了一种用液相色谱-串联质谱法(LC-MS/MS)测定农产品中氟蚁腙的简单方法。样品用磷酸匀浆,并用丙酮萃取。取一份粗提物用己烷和饱和氯化钠溶液再萃取。对于茶叶,在用己烷再萃取之前,先用氯化铵和磷酸进行固化处理。使用硅胶微型柱(500 mg)进行净化。在C18柱上进行LC分离,以含10 mM乙酸铵的甲醇-水(8:2)为流动相,并采用正离子电喷雾电离进行MS检测。氟蚁腙的校准曲线在0.002-0.2 µg/mL之间呈线性。在10种添加了0.01 µg/g(菠萝为0.05 µg/g)氟蚁腙的农产品中,氟蚁腙的回收率(n=5)为82-110%,其相对标准偏差为2-12%。

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