QuEChERS-超高效液相色谱-串联质谱法同时测定棕榈油中13种农药残留

Simultaneous determination of 13 kinds of pesticides residues in palm oil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法、棕榈液油、棕榈仁油、农药残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  palm olein  palm stearin  pesticide residue

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定棕榈油中氯酞酸、草芽畏、茅草枯等13种农药残留的定量分析方法。方法 棕榈油样品在柠檬酸体系下, 经乙腈提取, 用十八烷基硅烷(C18)除脂净化, 采用三重四级杆液质联用仪进行检测, 外标法定量。以5 mmol/L乙酸铵水溶液-甲醇为流动相, 梯度洗脱, 用Kinetex C18色谱柱(100 mm×4.6 mm, 2.6 μm)分离, 多反应监测模式, 电喷雾离子源(electrospray ionization source, ESI)正离子模式和负离子同时扫描。结果 在棕榈油和棕榈仁油2种食品基质中, 13种农药在浓度范围内线性关系良好, 相关系数大于0.990, 检出限为0.003 mg/kg, 定量限为0.01 mg/kg。方法验证实验对棕榈液油、棕榈仁油进行了3个不同加标水平, 结果表明2种基质的13种农药的回收率范围分别为71.0%~112.0%、80.1%~108.5%, 相对标准偏差均小于15%, 棕榈液油和棕榈仁油的精密度范围分别为1.0%~9.3%、1.6%~8.8%, 日间精密度范围分别为2.9%~15.6%和2.6%~9.3%。结论 该方法前处理简便、灵敏度高、准确性好, 适用于棕榈油中13种农药残留的定性筛查和准确定量, 为进出口食品提供检测依据。

英文摘要:

      Objecive To establish a method for the quantitative determination of 13 kinds of pesticide residues, including chlorothalonil, chlorpropham and diquat, in palm oil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Palm oil samples were extracted with acetonitrile in a citric acid system. This method employed octadecylsilane-bonded silica gel (C18) for defatting purification. This study employed liquid chromatography-tandem mass spectrometry for detection, with external standard quantification. Using a 5 mmol/L ammonium acetate aqueous solution-methanol mixture as the mobile phase, perform gradient elution. Chromatographic separation was performed using a Kinetex C18 column (100 mm×4.6 mm, 2.6 μm), multi-reaction monitoring mode. The electrospray ionization source (ESI) simultaneously scaned the positive ion mode and negative ions. Results In 2 kinds of food matrices—palm oil and palm kernel oil, 13 kinds of pesticides exhibited good linear relationships within their respective concentration ranges and the correlation coefficient was greater than 0.990. The limit of detection was 0.003 mg/kg, and the limit of quantitation was 0.01 mg/kg. Method validation experiments were conducted on palm oil and palm kernel oil at 3 different spiked levels. The results showed that the recovery rates of 13 kinds of pesticides on the 2 kinds of substrates ranged from 71.0% to 112% and 80.1% to 108.5%, respectively. With relative standard deviations all below 15%. The intraday precision ranges for palm oil and palm kernel oil were 1.0%–9.3% and 1.6%–8.8%, and the daytime precision ranges were 2.9%–15.6% and 2.6%–9.3%, respectively. Conclusion This method features simple pretreatment, high sensitivity, and good accuracy, making it suitable for the qualitative screening and precise quantitative analysis of 13 kinds of pesticide residues in palm oil. It provides a testing basis for food imports and exports.