食品科学 ›› 2010, Vol. 31 ›› Issue (12 ): 212-214.doi: 10.7506/spkx1002-6630-201012049

• 分析检测 • 上一篇    下一篇

液质法测定猪肉中八种糖皮质激素残留

牛晋阳,时宏霞   

  1. 中国肉类食品综合研究中心
  • 收稿日期:2010-01-26 出版日期:2010-06-15 发布日期:2010-12-29

Determination of Glucocorticoid Residues in Pork by HPLC-MS/MS

NIU Jin-yang, SHI Hong-xia   

  1. China Meat Research Center, Beijing 100068, China
  • Received:2010-01-26 Online:2010-06-15 Published:2010-12-29

摘要:

建立猪肉中糖皮质激素多残留的液相色谱串联质谱(LC-MS/MS)分析方法。样品经甲醇提取,固相萃取柱净化后采用LC-MS/MS 进行检测分析。对样品前处理条件和质谱参数进行研究,这些激素的物质的线性范围均为0.5~100μg/kg。低、中、高3 种质量浓度加标回收率均为78%~101%;最低检出限为0.2~2μg/kg。该方法快速简便,灵敏度高,选择性好,测定结果令人满意,可在各食品检测机构推广应用。

关键词: 糖皮质激素, 猪肉, 液相色谱- 串联质谱

Abstract:

A sensitive and rapid method using HPLC-MS/MS was proposed for the determination of 8 glucocorticoid residues in pork. Samples were extracted with methanol and cleaned up on a solid-phase extraction column before HPLC-MS/MS analysis. Optimum sample pretreatment conditions and mass spectral parameters were investigated. Calibration curves for 8 glucocorticoids showed good linearity over the concentration range from 0.5 to100μg/kg. Average recoveries for them spiked at 3 levels were between 78% and 101%. The method developed exhibited a limit of detection for all the analytes ranging from 0.2 to 2μg/kg. The determination of real samples was carried out using this method and satisfying results were obtained. This method is simple, rapid, sensitive and highly selective and is worth popularizing among food inspection organizations.

Key words: glucocorticoid, pork, HPLC-MS/MS

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