QuEChERS-超高效液相色谱-串联质谱法同时测定苦水玫瑰中6种氨基甲酸酯类及3种烟碱类杀虫剂
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(甘肃省疾病预防控制中心,甘肃 兰州 730020)

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张琳 女 主管技师 研究方向为理化检验 E-mail:1810585324@qq.com 谢迎春 女 主管技师 研究方向为理化检验 E-mail:86318740@qq.com

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Determination of 6 kinds of carbamate pesticides and 3 kinds of chloronicotinyl pesticides in Chinese Kushui rose by ultra high performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS
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(Gansu Provincial Center for Disease Control and Prevention, Gansu Lanzhou 730020, China)

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    摘要:

    目的 建立QuEChERS-超高效液相色谱-串联质谱同时测定苦水玫瑰中6种氨基甲酸酯类及3种烟碱类杀虫剂的方法。方法 苦水玫瑰样品粉碎后乙腈超声提取,经过QuEChERS分离净化后通过C18色谱柱(2.1 mm×100 mm,1.7 μm),以含0.1%甲酸的10 mmol/L乙酸铵-乙腈溶液进行梯度洗脱,采用电喷雾电离正离子(ESI+)多反应监测(MRM)模式检测,外标法定量。结果 9种农药在0.01~0.50 μg/mL浓度范围内线性相关系数(r)>0.990,加标回收率为76.3%~102%,相对标准偏差(RSD)为1.3%~9.0%(n=6),方法检出限和定量限分别为0.001 6~0.003 2和0.005 4~0.010 mg/kg。结论 本方法可以快速、简单、准确的同时检测苦水玫瑰中6种氨基甲酸酯类和3种烟碱类杀虫剂,适用于日常苦水玫瑰的检测。

    Abstract:

    Objective To establish a method for determination of 6 kinds of carbamate pesticides and 3 kinds of chloronicotinyl pesticides in Chinese Kushui rose by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) coupled with QuEChERS. Methods After extracted by acetonitrile, the Chinese Kushui rose was cleaned by QuEChERS. The target compounds were separated by C18 column(2.1 mm×100 mm,1.7 μm) using 10 mmol/L ammonium acetate solution (0.1% formic acid) with acetonrtrile as mobile phase for gradient elution, and analyzed by MS/MS system with electrospray ionization(ESI+) under muti-reaction monitoring mode and quantified by external standard method. Results All the 9 kinds of pesticides showed good linear relationships in range of 0.01-0.50 μg/mL, and the correlation coefficients were above 0.990, the recoveries at different spiked levels for all target compounds in blank matrices were 76.3%-102%,and the relative standard deviation (RSD)were 1.3%-9.0%(n=6). The limits of detection and quantification of the method were 0.001 6-0.003 2 and 0.005 4-0.010 mg/kg. Conclusion The method was suitable for rapid screening and analysis of 9 pesticide residues in Chinese Kushui rose with the advantage of accuracy, rapidity, simplicity and high sensitivity.

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张琳,骆姗,侯言东,李拥军,孙建云,谢迎春. QuEChERS-超高效液相色谱-串联质谱法同时测定苦水玫瑰中6种氨基甲酸酯类及3种烟碱类杀虫剂[J].中国食品卫生杂志,2020,32(5):514-518.

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  • 收稿日期:2020-08-06
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  • 在线发布日期: 2020-11-18
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