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    超高效液相色谱-串联质谱法测定鸡蛋中农药及其代谢物的含量

    Determination of Pesticides and Their Metabolites in Eggs by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

    • 摘要: 提出了超高效液相色谱-串联质谱法同时测定鸡蛋中多种农药及其代谢物含量的方法。将2.0 g鸡蛋样品用10 mL乙腈低温超声提取10 min,加入2.0 g无水硫酸钠和1.0 g氯化钠后离心。取2 mL上清液用QuEChERS吸附剂(25 mg C18)净化,取1.0 mL净化液过Oasis® PRiME HLB固相萃取小柱,收集流出液,用10%(体积分数)乙腈溶液稀释至2.0 mL。所得溶液采用Waters Acquity UPLC® BEH C18色谱柱分离,用不同体积比的乙腈和0.1%(体积分数)甲酸溶液作为流动相进行梯度洗脱,质谱分析采用电喷雾离子源正离子(ESI+)模式和多反应监测(MRM)模式,以特征离子和保留时间定性,标准曲线外标法定量。结果表明:农药及其代谢物标准曲线的线性范围均为0.5~20.0 μg·L-1,检出限(3S/N)为0.038 1~0.893 μg·kg-1。按标准加入法进行回收试验,回收率为74.0%~128%,测定值的相对标准偏差(n=6)为0.54%~10%。

       

      Abstract: A method for simultaneous determination of several pesticides and their metabolites in eggs by ultra-high performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS) was proposed. The egg sample (2.0 g) was extracted for 10 min with 10 mL of acetonitrile by ultrasound at low temperature, and then centrifuged after adding 2.0 g of anhydrous sodium sulfate and 1.0 g of sodium chloride. 2 mL of the supernatant was purified with QuEChERS adsorbent containing 25 mg of C18, and 1.0 mL of the purification solution was passed through Oasis® PRiME HLB solid phase extraction column. The effluent was collected and diluted to 2.0 mL with 10% (volume fraction) acetonitrile solution. The obtained solution was separated on a Waters Acquity UPLC® BEH C18 column, and gradient elution was performed using acetonitrile and 0.1% (volume fraction) formic acid solution at different volume ratios as mobile phase. ESI+ mode and MRM mode were adopted in MS analysis. Characteristic ions and retention time were used for qualitative analysis and standard curve external standard method was used for quantitative analysis. As shown by the results, linear ranges of the standard curves of pesticides and its metabolites were all 0.5-20.0 μg·L-1, with detection limits (3S/N) in the range of 0.038 1-0.893 μg·kg-1. Test for recovery was carried out according to the standard addition method, giving results in the range of 74.0%-128%, with RSDs (n=6) of the determined values in the range of 0.54%-10%.

       

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