| 气相色谱-串联质谱法检测乙氧氟草醚、唑草酮和乙螨唑在4种香辛料中的残留 |
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| 引用本文： | 焦斌,徐军,贾爽爽,吴小虎,刘新刚,董丰收,郑永权.气相色谱-串联质谱法检测乙氧氟草醚、唑草酮和乙螨唑在4种香辛料中的残留[J].农药学学报,2019,21(1):97-104. |
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| 作者姓名： | 焦斌 徐军 贾爽爽 吴小虎 刘新刚 董丰收 郑永权 |
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| 作者单位： | 中国农业科学院 植物保护研究所，北京 100193 |
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| 基金项目： | 农业行业标准制修订项目（2130109） |
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| 摘 要： | 建立了气相色谱-三重四极杆串联质谱 (GC-MS/MS)检测留兰香、桂皮、薄荷和月桂叶中乙氧氟草醚、唑草酮、乙螨唑残留的分析方法。4种香辛料用超纯水饱和，乙腈提取，无水硫酸镁及氯化钠盐析，氨基/石墨化碳黑 (NH2-Carb) 固相萃取柱净化，多反应监测模式，气相色谱-串联质谱测定。结果表明:乙氧氟草醚在0.002 5~2 mg/L范围内，唑草酮和乙螨唑在0.01~2 mg/L范围内，3种农药的进样质量浓度与对应的峰面积间呈良好的线性关系，r > 0.99；乙氧氟草醚在0.025、0.5和2 mg/kg 3个添加水平下，在4种香辛料中的平均回收率在86%~112%之间，相对标准偏差 (RSD)在2.4%~9.6%之间；唑草酮在0.2、0.5和2 mg/kg 3个添加水平下的平均回收率在87%~114%之间，RSD在2.4%~11%之间；乙螨唑在0.5、2和5 mg/kg 3个添加水平下的平均回收率在86%~116%之间，RSD在3.2%~11%之间。乙氧氟草醚、唑草酮和乙螨唑在4种香辛料中的定量限 (LOQ) 分别为0.025、0.2和0.5 mg/kg。
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| 关 键 词： | 气相色谱-串联质谱 乙氧氟草醚 唑草酮 乙螨唑 香辛料 残留 |
| 收稿时间： | 2018/10/15 0:00:00 |
Determination of oxyfluorfen, carfentrazone-ethyl and etoxazole residues in four spices using gas chromatography-tandem mass spectrometry |
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| JIAO Bin,XU Jun,JIA Shuangshuang,WU Xiaohu,LIU Xingang,DONG Fengshou and ZHENG Yongquan.Determination of oxyfluorfen, carfentrazone-ethyl and etoxazole residues in four spices using gas chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2019,21(1):97-104. |
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| Authors: | JIAO Bin XU Jun JIA Shuangshuang WU Xiaohu LIU Xingang DONG Fengshou and ZHENG Yongquan |
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| Institution: | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China |
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| Abstract: | An analytical method was developed for the determination of oxyfluorfen, carfentrazone-ethyl and etoxazole in Mentha spicata L, Cinnamomum cassia Presl, Mentha piperita L, and Laurus nobilis L using gas chromatography-tandem mass spectrometry (GC-MS/MS). The spice matrices were hydrated by ultrapure water, extracted by acetonitrile followed by the salting out process with anhydrous magnesium sulfate and sodium chloride then purified using the NH2-Carb column and determined by the GC-MS/MS under MRM mode. The calibration curve showed a good linearity in the range of 0.0025-2 mg/L (oxyfluorfen) and 0.01-2 mg/L (carfentrazone-ethyl and etoxazole), with the correlation efficient above 0.99. The average recoveries of oxyfluorfen in the four kinds of matrices at three spiked levels of 0.025, 0.5 and 2 mg/kg ranged from 86% to 112%, with the relative standard deviation (RSD) between 2.4%-9.6%. The average recoveries of carfentrazone-ethyl at three spiked levels of 0.2, 0.5 and 2 mg/kg ranged from 87% to 114%, with the RSD between 2.4%-11%. The average recoveries of etoxazole at three spiked levels of 0.5, 2 and 5 mg/kg ranged from 86% to 116%, with the RSD between 3.2%-11%. The limit of quantitation (LOQ) of oxyfluorfen, carfentrazone-ethyl and etoxazole in the four spices were 0.025, 0.2 and 0.5 mg/kg, respectively. |
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| Keywords: | gas chromatography-tandem mass spectrometry (GC-MS/MS) oxyfluorfen carfentrazone-ethyl etoxazole spices residue |
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