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臺灣農業化學與食品科學 Scopus

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篇名 利用QuEChERS萃取方法配合液相層析串聯質譜儀進行動物源性 食品中氯黴素類藥物之檢驗方法開發
卷期 55:5/6
並列篇名 Method Development for Analyzing Amphenicols in Animal Origin Foods Using QuEChERs and LC-MS/MS
作者 陳浩民於柏伸黃志能廖家鼎高雅敏周秀冠陳惠芳
頁次 236-248
關鍵字 氯黴素類藥物液相層析串聯質譜儀QuEChERs動物源性食品AmphenicolsLiquid chromatography/tandem mass spectrometer Animal origin foodsScopusTSCI
出刊日期 201710
DOI 10.6578/TJACFS.201710_55(5&6).0003

中文摘要

本研究利用QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)前處理技術配合液相層析串聯質譜 儀(LC/MS/MS),分析動物源性食品中(含雞蛋、魚肉、蜂蜜、牛乳、豬肉、豬肝及豬腎)之氯黴素、甲磺氯黴 素、氟甲磺氯黴素及氟甲磺氯黴素胺等4項氯黴素類藥物。檢體利用含1%醋酸之乙腈溶液進行初步萃取後, 以QuEChERS套組(含硫酸鎂、氯化鈉、檸檬酸鈉及檸檬酸氫二鈉半水結晶鹽)及分散型粉劑(含一級二級胺、 C18及無水硫酸鎂)進行鹽析及淨化處理。檢液經由氮氣濃縮後,以25%甲醇溶液回溶,利用Poroshell PFP管柱 以含5 m从醋酸銨之去離子水及含5 m从醋酸銨之甲醇溶液進行梯度沖提,並配合串聯質譜儀進行分析,定量上 採用內標校正後之基質匹配檢量線。本研究所有基質中,添加氯黴素0.05、0.1、0.25 ^g/知濃度下,平均回收 率介於84.5〜111.3%,變異係數小於14% ;添加甲磺氯黴素、氟甲磺氯黴素及氟甲磺氯黴素胺10、25及50 ^g/知 濃度下,平均回收率介於86.5〜111.4%,變異係數小於20%。本方法氯黴素定量極限介於0.05〜0.25 ;甲磺 氯黴素及氟甲磺氯黴素定量極限為1 ;氟甲磺氯黴素胺定量極限介於5〜25 ^g/知。

英文摘要

This study presents an analytical method using liquid chromatography/tandem mass spectrometer (LC/MS/ MS) in multiple reaction monitoring (MRM) mode and QuEChERs preatment for chromphenicol, thiamphenicol, florfenicol and florfenicol amine in animal origin foods (chicken egg, fish muSCCle , honey, milk, pork, pig liver and pig kidney). Homogenized sample was extracted with acetonitrile containing 1% acetic acid and then salted out with QuEChERs extraction powder, which is composed of magnesium sulfate, sodium chloride, sodium citrate and disodium citrate sesquihydrate. After centrifugation, the supernatant was cleaned up by primary secondary amine (PSA), C18 and magnesium sulfate. The extracts were concentrated under nitrogen stream and reconstituted into a methanol/Milli-Q water mixture (1:3, v/v) solution. The LC separation was conducted by an Poroshell PFP Column (2.7 "m, 3.0 x 100 mm) with gradient elution of 5 mm ammonium acetate in Milli-Q water and 5 mm ammonium acetate in methanol as the mobile phase. Matrix-match calibration curve normalized by internal standard was used to quantify for four amphenicols in this study. The recoveries of chloramphenicol (0. 05, 0.1 and 0.25 ^g/kg) spiked in all matrices ranged from 84.5 to 111.3%, and the coefficients of variation were below 14%. For thiamphenicol, florfenicol and florfenicol amine (10, 25 and 50 jug/kg) spiked in all matrices, recoveries ranged from 86.5 to 111.4%, and the coefficients of variation were below 20%. In all matrices, the limit of quantitation for chloramphenicol were between 0.05 to 0.25 ug/kg, for thiamphenicol and flofenicol were 1 Ug/kg, and for florfenicol amine were between 5 to 25 ug/kg.

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