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动物可食性组织中克拉维酸残留HPLC-MS/MS检测方法
引用本文:李帅鹏,黄显会,杨刚,郭春娜. 动物可食性组织中克拉维酸残留HPLC-MS/MS检测方法[J]. 中国农业科学, 2013, 46(23): 5012-5019. DOI: 10.3864/j.issn.0578-1752.2013.23.018
作者姓名:李帅鹏  黄显会  杨刚  郭春娜
基金项目:2010 年农业行业标准制修订项目(201012147)
摘    要:【目的】建立动物可食性组织中克拉维酸残留检测的高效液相色谱-串联质谱方法。【方法】1 g组织样品用3 mL 0.01 mol•L-1乙酸铵和3 mL乙腈提取后,经二氯甲烷反相提取净化,取水相定容到4 mL,正己烷除脂后上机检测。流动相为乙腈和0.1%甲酸水,梯度洗脱,经Luna 5μ C8色谱柱分离,采用电喷雾电离,多反应监测负离子模式对克拉维酸进行定量分析。【结果】采用基质匹配法对组织中克拉维酸的含量进行标准校正,克拉维酸质量浓度在5—500 μg•L-1范围内与峰面积间呈现良好的线性关系(r>0.999);组织中加标样品的检出限(按信噪比S/N≥3计)为10 μg•kg-1,定量限(按信噪比S/N≥10计)为20 μg•kg-1。在定量限、1/2最高残留限量、最高残留限量、2倍最高残留限量4个添加水平下,组织中克拉维酸的平均回收率为76.39%—89.26%,日间相对标准偏差为1.89%—6.20%。【结论】该方法可用于动物可食性组织中克拉维酸残留的分析检测。

关 键 词:高效液相色谱-串联质谱   克拉维酸   可食性组织   残留
收稿时间:2013-05-13

Determination of Clavulanic Acid Residue in Edible Tissues of Animals by High Performance Liquid Chromatography-Tandem Mass Spectrometry
LI Shuai-Peng,HUANG Xian-Hui,YANG Gang,GUO Chun-Na. Determination of Clavulanic Acid Residue in Edible Tissues of Animals by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Scientia Agricultura Sinica, 2013, 46(23): 5012-5019. DOI: 10.3864/j.issn.0578-1752.2013.23.018
Authors:LI Shuai-Peng  HUANG Xian-Hui  YANG Gang  GUO Chun-Na
Affiliation:National Reference Laboratory of Veterinary Drug Residues,College of Veterinary Medicine,South China Agricultural University,Guangzhou 510642
Abstract:【Objective】A confirmatory method was developed for the determination of clavulanic acid (CLAV) residue in edible tissues of animals by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). 【Method】 One gram tissues were extracted by 3 mL 0.01 mol•L-1 ammonium acetate solution and 3 mL acetonitrile,a back-extraction of the acetonitrile with dichloromethane,aqueous layer was diluted to 4mL,and the sample was determined by HPLC-MS/MS after defatted with N-hexane. The chromatographic separation was achieved on a Luna 5μ C8 column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. The identification of CLAV was carried out by MS/MS equipped with electrospray ionization in negative scanning and multiple reaction monitoring (MRM) modes. 【Result】Matrix-matched calibration standard was used for the quantification. Good linearity was achieved with correlation coefficients more than 0.999 for all analytes in the concentration of 5-500 μg•L-1. The limit of detection (LOD,S/N≥3) was 10 μg•kg-1 in tissues, and the limit of quantification (LOQ,S/N≥10) was 20 μg•kg-1. The mean recoveries at the four spiked levels of LOQ, 1/2MRL (the maximum residue limit), MRL and 2MRL were in the range of 76.39%-89.26% , with the inter-day relative standard deviations (RSD) of 1.89%-6.20%. 【Conclusion】In conclusion, the established method can be applied for the determination of CLAV residues in edible tissues of animals.
Keywords:high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)    clavulanic acid    edible tissues    residue
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