超高效液相色谱-串联质谱法测定稻田水产品中毒死蜱残留

以QuEChERS作为样品前处理手段,采用超高效液相色谱-串联质谱(UPLC-MS/MS)检测技术,建立了稻田水产品中毒死蜱残留的检测方法。样品经乙腈提取,由0.2 g乙二胺- N -丙基硅烷(PSA)和1.2 g无水硫酸镁分散萃取净化,采用Hypersil GOLD C 18 色谱柱(100 mm×2.1 mm, 5 μm)进行分离,用加热大气压电喷雾电离源、正离子模式进行扫描,在选择反应监测模式下检测,基质匹配标准曲线外标法定量。结果表明,毒死蜱在0.5~100.0 μg/L 范围内线性关系良好,相关系数大于0.999;毒死蜱的加标回收率为86.2%~103.6%,相对标准偏差为3.5%~7.6%( n =6),检出限为0.25 μg/kg ,定量限为0.5 μg/kg 。该方法简单、快速、灵敏,能够满足稻田水产品中毒死蜱残留的检测需求。

Determination of chlorpyrifos residues in the paddy field aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

A method was developed for the determination of chlorpyrifos residues in paddy field aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with acetonitrile and purified by using 0.2 g primary secondary amine (PSA) sorbent and 1.2 g MgSO₄. The target compound was separated on a Hypersil GOLD C₁₈ column (100 mm×2.1 mm, 5 μm), and was determined using a heated electrospray ionization (HESI) source in the positive ion selective reaction monitoring (SRM) mode. The analyte was quantified with external standard using the matrix-matched standard calibration curve method. The results showed that good linearities were obtained in the range of 0.5-100.0 μg/L, and the correlation coefficients were greater than 0.999. The spiked recoveries of chlorpyrifos ranged from 86.2% to 103.6% with RSDs of 3.5%-7.6% (n=6). The limits of detection and quantification were 0.25 μg/kg and 0.5 μg/kg, respectively. This method is simple, quick, sensitive, and suitable for the rapid determination and analysis of chlorpyrifos residues in paddy field aquatic products.