气相色谱串联质谱法分析虾中氯霉素

[Analysis of chloramphenicol in shrimps by gas chromatography tandem mass spectrometry].

作者信息

Yang Xin, Zhou Rui, Zhao Yun-Feng, Wu Yong-Ning

机构信息

National Institute of Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China.

出版信息

Wei Sheng Yan Jiu. 2005 Sep;34(5):584-7.

PMID:16329603

Abstract

OBJECTIVE

A sensitive method based on isotope dilution gas chromatography tandem mass spectrometry is described for the determination of the antibiotic chloramphenicol (Cap) in shrimp tissue.

METHODS

Homogenized shrimp samples spiked with an isotopically labeled internal standard (d5-Cap) were extracted with ethyl acetate extraction, defatted with hexane, followed by a clean-up step on a SPE C18 cartridge, and then the elute was evaporated and derivatized with Sylon BFT {N,O-bis (trimethylsily) trifluoroacetamide[BSTFA]-trimethylchlorosilane [TMCS] ,99 + 1}. Analyzes were determined by GC/MS-MS in MRM mode.

RESULTS

Internal calibration curves obtained for Cap/ d5-Cap in the 5 to 500 pg range were linear with correlation coefficients of 0.9958. Limit of quantitation (LOQ) was 0.3ng/g. Shrimp tissues were fortified with Cap at 0.3, 0.5, 1.0 ng/g level, average recoveries were 104%, 111% and 95% , respectively.

CONCLUSION

The proposed method allows the detection, quantitation and confirmation of Cap in shrimps with high accuracy and sensitivity.

摘要

目的

描述一种基于同位素稀释气相色谱串联质谱法的灵敏方法，用于测定虾组织中的抗生素氯霉素（Cap）。

方法

将添加了同位素标记内标（d5-Cap）的虾匀浆样品用乙酸乙酯萃取，用己烷脱脂，然后在固相萃取C18柱上进行净化步骤，接着将洗脱液蒸发并用Sylon BFT{N,O-双（三甲基硅基）三氟乙酰胺[BSTFA]-三甲基氯硅烷[TMCS]，99 + 1}进行衍生化。采用气相色谱/质谱联用仪在多反应监测（MRM）模式下进行分析测定。