食品科学 ›› 2009, Vol. 30 ›› Issue (16): 235-239.doi: 10.7506/spkx1002-6630-200916051

• 分析检测 • 上一篇    下一篇

固相萃取-液相色谱串联质谱同时测定牛奶中8种甾类同化激素多残留

吕惠卿1,陈慧华2,韦敏珏2,应永飞2   

  1. 1. 浙江中医药大学药学院 2.浙江省畜产品质量安全检测中心
  • 收稿日期:2008-08-18 出版日期:2009-08-15 发布日期:2010-12-29
  • 通讯作者: 吕惠卿 E-mail:hzlhq@126.com
  • 基金资助:

    浙江省重大科技攻关项目(2006C12025)

Solid Phase Extraction Followed by Liquid Chromatography-Tandem Mass Spectrometry for the Simultaneous Determination of Eight Anabolic Steroids in Milk

LU Hui-qing1,CHEN Hui-hua2,WEI Min-jue2,YING Yong-fei2   

  1. (1. College of Pharmaceutical Sciences, Zhejiang Chinese Medical University, Hangzhou 310053, China;
    2. Animal Products Quality Testing Center of Zhejiang Province, Hangzhou 310020, China)
  • Received:2008-08-18 Online:2009-08-15 Published:2010-12-29
  • Contact: LU Hui-qing1, E-mail:hzlhq@126.com

摘要:

采用固相萃取- 液相色谱串联质谱仪(SPE-LC/MS),建立牛奶中8 种同化激素(睾酮、孕酮、诺龙、甲基睾酮、勃地龙、群勃龙、美雄酮、康力龙)多残留的快速测定方法。样品经叔丁基甲醚提取,过C18 固相萃取柱净化,氮吹至干,残留物用10% 甲醇- 水(10:90,V/V)溶解后测定。采用正离子扫描方式进行仪器方法学研究,确定监测离子对,进行MRM 模式定性定量分析。该方法的检出限(LOD)为0.2~0.5 μ g/L,定量限(LOQ)为0.5~1.0μg/L;在2.0~200.0μg/L 范围内线性关系良好(r > 0.9990)。在1.0 ~5.0μg/L 的添加水平上,8 种激素的平均回收率在59.1%~97.7% 之间,相对标准偏差(RSD)为3.2%~11.9%。该法操作简单、灵敏度高,可用于牛奶中8 种甾类同化激素的测定。

关键词: 固相萃取, 液相色谱-串联质谱, 甾类同化激素, 牛奶

Abstract:

This study developed a quick and specific method for the identification and trace quantification of 8 anabolic steroids (TS, PG, NT, MTS, BOL, TB, DIA, and STA) in milk. Samples were extracted using methyl tert-butyl ether, and the extracts were cleaned up by solid-phase extraction on a C18 (SPE) cartridge, blowed to dryness by nitrogen, and dissolved in a mixture of 10% methanol and water (10:90, V/V) prior to LC-MS/MS analysis in a multiple reaction monitoring (MRM) mode. The limits of detection (LODs) ranged in 0.2 - 0.5 μg/L, and the limits of quantification (LOQs) were between 0.5 and 1.0 μg/L. The regression equations were well linear between 2.0 and 200.0 μg/L for these steroids (r > 0.9990). The recoveries ranged from 59.1% to 97.7% with a RSD of 3.2%-11.9% (n = 3) at three spiked levels of 1.0-5.0 μg/L. The method is simple, sensitive and rapid and therefore can be used for the simultaneous determination of 8 anabolic steroids in milk.

Key words: solid-phase extraction, LC-MS/MS, anabolic steroids, milk

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