固相萃取-高效液相色谱-串联质谱联用测定竹笋中残留的7种杀虫剂农药

Determination of seven pesticide residues in bamboo shoots by high performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction

建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定竹笋中丁烯氟虫腈、毒死蜱、氯虫苯甲酰胺、氟虫腈、吡虫啉、茚虫威和辛硫磷7种农药残留的分析方法。样品用乙腈提取后,经PSA固相萃取小柱净化,采用AtlantisT3色谱柱分离,以0.1%甲酸水溶液(含5 mmol/L乙酸铵)和乙腈为流动相,梯度洗脱分离,在电喷雾离子源正、负离子模式下采用质谱多反应监测(MRM)模式检测。结果表明,7种农药在10～100μg/L范围内具有良好的线性关系(相关系数r为0.990 0～0.999 4);4、8、32μg/kg添加水平下的平均回收率为76.0%～102.6%;相对标准偏差为3.2%～11.0%;7种农药的检出限为0.02～0.5μg/kg,定量限为0.08～1.5μg/kg。该方法准确度、灵敏度高,简单、快速,可满足竹笋中7种杀虫剂残留同时检测的要求。

A simple and efficient method based on solid-phase extraction （SPE） and high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was developed for the determination of butylene fipronil, chlorpyrifos, chlorantraniliprole, fipronil, imidacloprid, indoxacarb and phoxim residues in bamboo shoots. The sample was extracted with acetonitrile and purified by a primary secondary amine （PSA） solid-phase extraction cartridge. The detec tion of targets was performed by HPLC-MS/MS with multiple reaction monitoring （MRM） mode. All the seven pesticides were completely separated in 15 rain with an excellent linear relationship. The limits of detection and the limits of quantification for the seven pesticides were 0.02 -0.5 μg/kg and 0.08 - 1.5 μg/kg, respectively. The recoveries of the seven pesticides spiked in a bamboo shoot sample at the levels of 4, 8, 32 ptg/kg were in the range from 76.0% to 102.6% （ the RSD ≤ 11.0%, n = 3）. The method was successfully applied to the real bamboo shoot samples. The method has high accuracy and sensitivity, and is simple and quick. It can meet the requirement of the sinmltaneous determination of the seven pesticides in bamboo shoots.