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超高效液相色谱-质谱法测定豆芽中多菌灵、2,4-二氯苯氧乙酸、恩诺沙星残留

Determination of Carbendazim, 2,4-D and Enrofloxacin Residues in Bean Sprouts by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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【作者】 丁丽曾绍东魏晓奕王明月李积华程盛华

【Author】 DING Li;ZENG Shao-dong;WEI Xiao-yi;WANG Ming-yue;LI Ji-hua;CHENG Sheng-hua;Agricultural Products Processing Research Institute, Chinese Academy of Tropical Agricultural Sciences;Laboratory of Quality and Safety Risk Assessment on Agro-products Processing,Ministry of Agriculture;

【机构】 中国热带农业科学院农产品加工研究所农业部农产品加工质量安全风险评估实验室

【摘要】 建立豆芽中多菌灵、2,4-二氯苯氧乙酸(2,4-dichlorophenoxyacetic acid,2,4-D)、恩诺沙星残留检测的超高效液相色谱-质谱的分析方法。样品经酸化乙腈提取,浓缩后经WAX小柱净化,采用Waters C18色谱柱分离,以甲醇和0.1%甲酸溶液为流动相进行梯度洗脱,采用电喷雾-正负离子多反应监测模式,外标法定量。在5~150μg/L的质量浓度范围内,各种添加剂相关系数均大于0.999 0,该方法的检出限在0.5μg/kg之间,定量限在1.5μg/kg之间。添加5.0、10.0μg/kg和25.0μg/kg三个不同水平时,多菌灵、2,4-D、恩诺沙星的回收率在80.4%~97.8%之间,日内和日间相对标准偏差在1.25%~5.47%之间。该方法简单、灵敏度高、分析时间短,适用于多菌灵、2,4-D、恩诺沙星的测定。

【Abstract】 A method was established for determining carbendazim, 2,4-D, enrofloxacin residues in bean sprouts by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS). Samples were extracted with acidified acetonitrile, and cleaned up on a WAX cartridge. The target analytes were separated on a Waters C18 column with gradient elution using a mobile phase made up of methanol and 0.1% formic acid. Detection was carried out using positive/negative electrospray ionization and multiple-reaction monitoring(MRM), and the external standard method was used for quantification. In the linear range of 5–150 μg/L, the correlation coefficients were all larger than 0.999 0 for carbendazim, 2,4-D and enrofloxacin. The limits of detection(LODs) were 0.5 μg/kg and the limits of quantitation(LOQs) were 1.5 μg/kg. The recovery rates at three spiked levels of 5.0, 10.0 and 25.0 μg/kg were in the range of 80.4%–97.8%. The relative standard deviation(RSD) of intra-day and inter-day assays was 1.25%–5.47%. The method proved to be simple, sensitive, rapid and suitable for the determination of carbendazim, 2,4-D and enrofloxacin residues in bean sprouts.

【基金】 农业部财政专项,农产品质量安全监管(风险评估)项目
  • 【分类号】O657.63;TS207.3
  • 【被引频次】33
  • 【下载频次】555
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