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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Rapid determination of chloramphenicol residues in milk powder by liquid chromatography-elektrospray ionization tandem mass spectrometry
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Rapid determination of chloramphenicol residues in milk powder by liquid chromatography-elektrospray ionization tandem mass spectrometry

机译：液相色谱-电喷雾串联质谱法快速测定奶粉中的氯霉素残留

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摘要

A simple and rapid liquid chromatography tandem mass spectrometry (LC-ESI-MS-MS) confirmation method for the analysis chloramphenicol (CAP) in milk powder has been developed. Samples were extracted by using liquid-iquid extraction steps with ethyl acetate. Lipids were removed using hexsan. LC separation was achieved by using a Phenomenex Luna C-18 column and acetonitryle-water as a mobile phase. The mass spectrometer was operated in multiple reaction monitoring mode (MRM) with negative electro-spray interface (ESI-). The four transitions were monitored m/z 321 -> 257, 321 -> 194, 321 -> 152, 326 -> 157 (IS) and for quantification, the transition m/z 321 -> 152 was chosen. Validation of the method was done according to criteria of Decision Commission No 2002/657 EC. Validation includes the determination of specification, linearity, precision (within- and between-day), accuracy, decision limit (CC(x) and detection capability (CC beta). Samples were fortified at CAP levels 0.30, 0.45 and 0.60 mu g/kg with CAP-5d as internal standard. The precision within-day (RSD%) was lower than 12% and accuracy (RE%) ranged from -9.8 to -3.7%. The precision between-day (RSD%) was less than 15%. The limit of decision (CC alpha) and detection capability (CC beta) for milk powder 0.09 and 0.11 mu g/kg. Value CC alpha and CC beta were calculated for the 321 -> 152 ion transition. This method has been successfully used for routine analysis. (C) 2008 Elsevier B.V. All rights reserved.
机译：开发了一种简单快速的液相色谱串联质谱（LC-ESI-MS-MS）确认方法，用于分析奶粉中的氯霉素（CAP）。通过使用乙酸乙酯的液-液萃取步骤萃取样品。使用己三酸去除脂质。使用Phenomenex Luna C-18色谱柱和乙腈-水作为流动相可实现LC分离。质谱仪在带有负电喷雾接口（ESI-）的多反应监测模式（MRM）下运行。通过m / z 321-> 257，321-> 194，321-> 152，326-> 157（IS）监测这四个转变，为进行定量，选择了m / z 321-> 152。该方法的验证是根据2002/657 EC号决策委员会的标准进行的。验证包括确定规格，线性，精度（日间和日间），准确性，决策极限（CC（x）和检测能力（CC beta）），样品的CAP含量分别为0.30、0.45和0.60μg / g。以CAP-5d为内标的千克，日内精度（RSD％）低于12％，精度（RE％）介于-9.8至-3.7％之间，日间精度（RSD％）小于15％。乳粉0.09和0.11μg/ kg的判定极限（CC alpha）和检测能力（CC beta）。计算了321-> 152离子跃迁的CC alpha和CC beta值。 （C）2008 Elsevier BV保留所有权利。

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