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。
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.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2014年第22期169-175,共7页
Food Science
基金
农业部财政专项
农产品质量安全监管(风险评估)项目
关键词
超高效液相色谱-质谱
多菌灵
2
4-D
恩诺沙星
残留
豆芽
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS)
carbendazim
2,4-D
enrofloxacin
residue
bean sprout
