食品科学 ›› 2010, Vol. 31 ›› Issue (2): 120-123.doi: 10.7506/spkx1002-6630-201002029

• 分析检测 • 上一篇    下一篇

液相色谱- 串联质谱法测定海产品中21 种磺胺类药物残留

孙玉增,徐英江,刘慧慧,张世娟,秦华伟,高继庆   

  1. 山东省海洋水产研究所
  • 收稿日期:2009-02-16 出版日期:2010-01-15 发布日期:2010-12-29
  • 通讯作者: 徐英江 E-mail:xu_ying_jiang@sina.com
  • 基金资助:

    山东省科技攻关项目(2007GG20005001);国家海洋局海洋公益性行业科研专项经费项目(200805031)

Simultaneous Determination of 21 Sulfonamide Residues in Aquatic Products by Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

SUN Yu-zeng,XU Ying-jiang,LIU Hui-hui,ZHANG Shi-juan,QIN Hua-wei,GAO Ji-qing   

  1. (Shandong Provincial Marine Fisheries Research Institute, Yantai 264006, China)
  • Received:2009-02-16 Online:2010-01-15 Published:2010-12-29
  • Contact: XU Ying-jiang, E-mail:xu_ying_jiang@sina.com

摘要:

研究一种能够同时测定水产品中21 种磺胺类药物残留量的检测方法——超高效液相色谱质谱法。样品经乙酸乙酯提取,经固相萃取小柱净化,氮气吹干后,用1mL 流动相定容残余物。采用ACQUITYTM BEH C18 色谱柱,用甲醇和5mmol/L 乙酸铵溶液(含体积分数0.1% 甲酸)作流动相,采用质谱技术分析。结果表明,检出限为0.01~0.20μg/kg,定量限为0.03~0.67μg/kg,平均回收率为68%~82%,相对标准偏差为4.1%~11.8%。该方法适合水产品中多种磺胺类药物的检测。

关键词: 液相色谱- 串联质谱(UPLC-MS/MS), 水产品, 磺胺类药物

Abstract:

An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometric (UPLC-MS/MS) method has been developed for the simultaneous determination of 21 sulfonamide residues in aquatic products. Samples were extracted with ethyl acetate, cleaned up using an HLB SPE cartridge and blown to dryness under nitrogen, and the residues were then dissolved in 1 mL of mobile phase. The 21 analytes were separated on ACQUITYTM BEH C18 column with a mobile phase composed of methanol and 5 mmol/L aqueous ammonium acetate solution (containing 0.1% formic acid). The limits for qualitative detection and quantitative determination were 0.01-0.20μg/kg and 0.03-0.67 μg/kg, respectively. The average recoveries at three spike levels ranged 68%-82%, with RSDs ranging 4.1%-11.8%. All these figures of merit demonstrate a good suitability of this method for the simultaneous determination of sulfonamide residues in aquatic products.

Key words: UPLC-MS/MS, aquatic products, sulfonamide residues

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