超高效液相色谱-串联质谱法检测桃中13种高关注农药残留

Detection of 13 kinds of highly attentive pesticides residues in peach by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  桃  农药残留  超高效液相色谱-串联质谱法

英文关键词:peach  pesticides residues  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定桃中13种高关注农药残留的分析方法。方法 样品采用含1%(体积分数)乙酸的乙腈溶液超声提取, 4 g无水硫酸镁和1 g氯化钠盐析后, 不净化, 直接经Waters HSS T3 (2.1 mm×100 mm, 1.8 μm)色谱柱分离, 用甲醇和2 mmol/L甲酸铵水溶液为流动相梯度洗脱, 串联质谱电喷雾正离子扫描, 多反应监测模式检测, 基质匹配标准溶液-外标法定量。结果 13种农药在0.5~8 μg/kg范围内线性关系良好, 相关系数r均大于0.997, 在桃中添加0.5、2和5 μg/kg 3个浓度的农药标准溶液, 平均回收率为63.2%~123.0%, 日内相对标准偏差(relative standard deviation, RSD)为0.6%~10.3% (n=6), 日间RSD为2.8%~13.2% (n=3), 定量限均为0.5 μg/kg。结论 该方法简单、可靠、灵敏, 适用于桃中13种农药残留的检测。

英文摘要:

      Objective To establish a rapid method for the simultaneous detection of 13 kinds of highly attentive pesticides residues in peach by ultra performance liquid chromatography-tandem mass spectrometry. Methods The peach samples were extracted by ultrasonic extraction with acetonitrile containing 1% acetic acid, followed by salting out with 4 g magnesium sulfate and 1 g sodium chloride without further cleanup, then separated on a Waters HSS T3 (2.1 mm×100 mm, 1.8 μm) column by gradient elution with methanol and 2 mmol/L ammonium formate as mobile phase, ionized with positive electrospray ionization, detected under multiple reaction monitoring mode, and quantified with matrix-matched external standard calibration curves. Results There existed good linearities for 13 kinds of pesticides in the concentration range of 0.5?8 μg/kg, with correlation coefficients higher than 0.997. The average recoveries at three spiked levels of 0.5, 2 and 5 μg/kg in peach ranged from 63.2% to 123.0%, with intra-day relative standard deviations (RSD) of 0.6%?10.3% (n=6) and inter-day RSD of 2.8%?13.2% (n=3). The limits of quantification for all the analytes were 0.5 μg/kg. Conclusion The proposed method is simple, accurate and sensitive, which is suitable for the detection of 13 kinds of pesticide residues in peach.