Abstract

A novel method for the determination of pyrethroid pesticide residues in wooden toys was developed. Wooden toy samples were extracted with petroleum ether−acetone (1 : 1, v/v), cleaned up on a florisil solid phase extraction cartridge and determined by gas chromatography equipped with electron capture detector (GC−ECD), followed by validation using gas chromatography−mass spectrometry (GC−MS) with negative chemical ionization. Calibration curves were linear in the range of 0.02–0.5 mg/kg with correlation coefficients exceeding 0.9975 for GC−ECD and GC−MS. At spiked concentrations of 0.1, 0.2 and 0.5 mg/kg, the average recoveries and relative standard deviations were 82–97% and 1.5–7.8%, respectively. The limit of quantification for each analyte was 0.1 mg/kg, which satisfied the current maximum residue limit permitted in wooden toys. Results also showed that the developed method could be successfully applied to determine permethrin, cypermethrin, cyfluthrin, deltamethrin residues in real wooden toy samples.

中文翻译：

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气相色谱和气相色谱-质谱法测定木制玩具中的拟除虫菊酯残留

摘要

建立了测定木制玩具中拟除虫菊酯类农药残留的新方法。用石油醚-丙酮（1：1，v / v）提取木制玩具样品，在弗洛里西尔固相提取柱上纯化，并通过配备电子捕获检测器（GC-ECD）的气相色谱法测定，然后使用气体进行验证色谱-质谱（GC-MS）具有负化学电离作用。校正曲线在0.02–0.5 mg / kg范围内呈线性，对于GC-ECD和GC-MS，相关系数超过0.9975。加标浓度为0.1、0.2和0.5 mg / kg时，平均回收率和相对标准偏差分别为82–97％和1.5–7.8％。每个分析物的定量限为0.1 mg / kg，满足了目前木制玩具中允许的最大残留限量。结果还表明，所开发的方法可以成功地用于测定实际木制玩具样品中的氯菊酯，氯氰菊酯，氟氰菊酯，溴氰菊酯残留量。