以改良式QuEChERS技術建立食品中磺胺劑、喹諾酮類、巨環類、四環黴素類、抗球蟲、抗原蟲等動物用藥殘留分析方法

Development and Validation of a Procedure for Determination of Veterinary Drug-sulfonamides, Quinolones, Antibiotics and Its Metabolite, Tetracyclines Antiprotozal Drugs, Ionophore Coccidiostats in Livestock and Poultry Products Using Modified QuEChERS Method and Liquid Chromatography/tandem Mass Spectrometry

林建安(Chien-An Lin) ； 廖伶莉(Ling-Li Liao) ； 陳婉玲(Wan-Ling Chen) ； 陳素娥(Su-O Chen)

《化學》 76卷1期 (2018/03) Pp. 87-101

https://doi.org/10.6623/chem.201803_76(1).001

摘要

食安事件議題近年頗受重視。縮短檢驗時效、提升檢驗量能，以確保食品安全與市民健康，是現行食安檢驗的重要課題。本研究嘗試以改良式QuEChERS前處理技術，整併多種動物用藥品項，進而有效縮短前處理流程。以含25 mM EDTA醋酸銨溶液(5 mM)及含5%甲酸乙腈溶液配製成具有緩衝性質之萃取溶劑，並選用EMR粉劑、食鹽、無水硫酸鈉及Ｃ18粉劑達到萃取、淨化之效果。在動物用藥品項，考量pKa性質及乙腈相溶性之因素，挑選磺胺劑及喹諾酮類抗生素共48項、抗生素及其代謝物16項、離子型抗球蟲、抗原蟲及四環黴素類等五大類動物用藥進行研究。本方法使用液相層析串聯質譜儀為分析儀器，分別使用0.1%甲酸溶液及0.1%甲酸乙腈溶液為移動相，分析管柱採用Chromolith High Resolution RP-C18 endcapped，150 × 4.6 mm，檢量線以前添加方式配製，標準品濃度為25～250 ng/g，R2均可達到0.995以上，方法之定量極限為12.5 ng/g。以定量極限2至10倍量添加至空白檢體(牛五花肉、雞肉)進行添加回收試驗，其平均回收率介於70-120%間，變異係數(小於10%)2.0～10%。實驗結果顯示，本分析方法穩定性佳，與公告方法搭配使用，將可提升檢驗效能。

關鍵字

動物用藥 ； 磺胺劑及喹諾酮類 ； 抗生素及其代謝物 ； 抗球蟲 ； 抗原蟲 ； 四環黴素 ； QuEChERS ； 液相層析串聯質譜儀

並列摘要

Food safety was the most concerned issue for the past few years. Shorter the experiment time but higher the efficiency was the most important topic to ensure the food safety and people health. This study was developed a modified QuEChERS method and liquid chromatography/ tandem mass spectrometry to shorter time-costing of analysis veterinary drugs. Sample preparation involves rapid protein precipitation and extraction by acidified acetonitrile and 25 mM EDTA in 5 mM ammonium acetate solution, followed by the use of EMR-Lipid dSPE and C18EC for cleanup. Consider pKa and acetonitrile solubility, this study was picked up five veterinary drug classes to research. The chromatographic was performed on a Chromolith High Resolution RP-C18 endcapped, 150 × 4.6 mm column using water and acetonitrile as mobile phases with 0.1% formic acid. This method was validated with bovine and chicken muscle. Greater than 95% of the drugs had linear regression coefficients (r) greater than 0.995, recoveries between 70 to 120%, and coefficient of variation (CV, n = 3, 12.5 ng/g spiking) within 10%. The result showed that the developed method was stable and it would higher the efficience of analysis with official multi-residue testing methods for veterinary drugs promulgated by the Ministry of Health and Welfare (MOHW) of Taiwan.

並列關鍵字

Multiclass veterinary drug ； Sulfonamide residues ； Quinolones ； Antibiotics and its metabolite ； Tetracyclines antiprotozal drugs ； Onophore coccidiostats ； QuEChERS ； LC-MS/MS