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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
引用本文:丁丽,曾绍东,魏晓奕,王明月,李积华,程盛华.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[J].食品科学,2014,35(22):169-175.
作者姓名:丁丽  曾绍东  魏晓奕  王明月  李积华  程盛华
作者单位:1.中国热带农业科学院农产品加工研究所,广东 湛江 524001; 2.农业部农产品加工质量安全风险评估实验室,广东 湛江 524001
基金项目:农业部财政专项;农产品质量安全监管(风险评估)项目
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5~150 μg/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0.5 μg/kg之间,定量限在1.5 μg/kg之间。添加5.0、10.0 μg/kg和25.0 μg/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。

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  

Determination of Carbendazim, 2,4-D and Enrofloxacin Residues in Bean Sprouts by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
DING Li,ZENG Shao-dong,WEI Xiao-yi,WANG Ming-yue,LI Ji-hua,CHENG Sheng-hua.Determination of Carbendazim, 2,4-D and Enrofloxacin Residues in Bean Sprouts by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Food Science,2014,35(22):169-175.
Authors:DING Li  ZENG Shao-dong  WEI Xiao-yi  WANG Ming-yue  LI Ji-hua  CHENG Sheng-hua
Affiliation:1. Agricultural Products Processing Research Institute, Chinese Academy of Tropical Agricultural Sciences, Zhanjiang 524001, China; 2. Laboratory of Quality and Safety Risk Assessment on Agro-products Processing, Ministry of Agriculture, Zhanjiang 524001, China
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.
Keywords:ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS)  carbendazim  2  4-D  enrofloxacin  residue  bean sprout
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