Food and Drug Administration, Ministry of Health and Welfare, Executive Yuan, 161-2 Kunyang St., Nangang Dist., Taipei City 11561, Taiwan.
J Food Drug Anal. 2019 Jul;27(3):703-716. doi: 10.1016/j.jfda.2019.02.004. Epub 2019 Mar 12.
In this study, we developed a novel analysis method based on liquid chromatography/tandem mass spectrometry (LC-MS/MS) to allow the simultaneous identification of 20 coccidiostats in eight matrix categories, including the muscles of chicken, swine, cow, and fish as well as chicken eggs, bovine milk, and porcine viscera. In the pretreatment procedure, acetonitrile/methanol (95:5, v/v) containing 1% formic acid, 5 g of sodium acetate, and 6.0 g of anhydrous magnesium sulfate was used for extraction, followed by a clean-up procedure using n-hexane saturated with ACN to facilitate the elimination of analytes from high lipid samples. Chromatographic separations were achieved using a Poroshell 120SB C18 column and operated with a gradient mobile phase system consisting of methanol (with 0.1% formic acid) and 5 mM ammonium formate, and the MS detection was monitored simultaneously. The method was validated in accordance with the Guidelines for the Validation of Food Chemical Methods by the Taiwan Food and Drug Administration. The limit of quantitation among 8 matrices were 0.5-2 ng g. The proposed method proved highly effective in detecting the presence of targeted veterinary drugs, providing a high degree of precision and accuracy over a broad range of matrices.
在本研究中,我们开发了一种基于液相色谱/串联质谱(LC-MS/MS)的新型分析方法,可同时鉴定 8 种基质类别中的 20 种抗球虫药,包括鸡肉、猪肉、牛肉和鱼肉以及鸡蛋、牛奶和猪内脏。在预处理过程中,使用含 1%甲酸的乙腈/甲醇(95:5,v/v)、5 g 醋酸钠和 6.0 g 无水硫酸镁进行提取,然后用乙腈饱和的正己烷进行净化处理,以利于从高脂肪样品中去除分析物。采用 Poroshell 120SB C18 柱进行色谱分离,采用甲醇(含 0.1%甲酸)和 5 mM 甲酸铵的梯度流动相系统进行操作,并同时进行 MS 检测。该方法按照台湾食品药品管理局的《食品化学方法验证指南》进行验证。在 8 种基质中,定量限为 0.5-2 ng/g。该方法在检测目标兽药方面非常有效,在广泛的基质范围内具有很高的精密度和准确度。