高效液相色谱-串联质谱法测定豆芽中恩诺沙星的含量

食品科学 ›› 2012, Vol. 33 ›› Issue (20): 180-183.

高效液相色谱-串联质谱法测定豆芽中恩诺沙星的含量

崔相勇1，张凤清1，周长民1，王岩松1，钟启智2

1.沈阳产品质量监督检验研究院 2.辽宁省公安厅

收稿日期:2011-07-22 修回日期:2012-08-06 出版日期:2012-10-25 发布日期:2012-11-09
通讯作者: 崔相勇 E-mail:305560343@163.com

Determination of Enrofloxacin in Soy Bean Sprout by LC-MS/MS

Received:2011-07-22 Revised:2012-08-06 Online:2012-10-25 Published:2012-11-09
Contact: Xiang-Yong CUI E-mail:305560343@163.com

摘要/Abstract

摘要： 采用高效液相色谱-质谱联用法测定豆芽中恩诺沙星的含量。样品经0.1mol/L NaOH溶液提取后，经Waters Oasis MAX阴离子交换柱净化，以双氟沙星为内标，采用反相高效液相色谱分离，以乙腈-水(含0.1%甲酸)为流动相进行梯度洗脱，通过带有电喷雾离子化源的串联质谱仪，应用正离子扫描，在多反应监测模式下进行定性与定量分析。本法线性范围为1～100μg/kg，平均回收率为91.6%～94.0%，相对标准偏差不大于6.6%，方法的检出限为0.3μg/kg。

关键词: 高效液相色谱-质谱联用, 恩诺沙星, 双氟沙星, 豆芽

Abstract: This paper reports a sensitive and specific LC-MS/MS method for the determination of enrofloxacin in soy bean sprout. Samples were extracted with 0.1 mol/L NaOH, cleaned up on a Waters Oasis MAX anion exchange column, and separated by RP HPLC using a mobile phase consisting of acetonitrile and 0.1% formic acid for gradient elution. Enrofloxacin was quantitatively and qualitatively analyzed by ESI-MS/MS in the positive ion scan MRM mode. The method showed a linear range of 1–100 μg/kg and a limit of detection of 0.3 μg/kg. The average spike recovery rates of enrofloxacin in blank sample was 91.6%–94.0% with RSD of 6.6%.

Key words: high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS), enrofloxacin, difloxacin, soy bean sprout

中图分类号:

崔相勇1，张凤清1，周长民1，王岩松1，钟启智2. 高效液相色谱-串联质谱法测定豆芽中恩诺沙星的含量[J]. 食品科学, 2012, 33(20): 180-183.

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