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Bithionol residue analysis in animal-derived food products by an effective and rugged extraction method coupled with liquid chromatography–tandem mass spectrometry
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-08-31 , DOI: 10.1016/j.jchromb.2017.08.035
Weijia Zheng , Jin-A Park , A.M. Abd El-Aty , Seong-Kwan Kim , Sang-Hyun Cho , Jeong-Min Choi , Hee Yi , Soo-Min Cho , H.A. El-Banna , Jae-Han Shim , Byung-Joon Chang , Jing Wang , Jin-Suk Kim , Ho-Chul Shin

Herein, we developed a simple analytical procedure for the quantitation of bithionol residues in animal-derived food products such as porcine muscle, eggs, milk, eel, flatfish, and shrimp using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography–electrospray ionization tandem mass spectrometry (LC-ESI+/MS-MS). Samples were extracted with 0.1% solution of formic acid in acetonitrile and the extract was purified using a C18 sorbent. Separation was performed on a Waters XBridge™ C18 reversed-phase analytical column using 0.1% solution of formic acid/acetonitrile as the mobile phase. Six-point matrix-matched calibration indicated good linearity, with the calculated coefficients of determination (R2) being ≥ 0.9813. Intra- and inter-day recoveries (determined at spiking levels equivalent to 1 × and 2 × the limit of quantitation (0.25 μg/kg)) ranged between 80.0 and 94.0%, with the corresponding relative standard deviations (RSDs) being ≤ 8.2%. The developed experimental protocol was applied to different samples purchased from local markets in Seoul, which were tested negative for bithionol residues. In conclusion, the proposed method proved to be versatile and precise, being ideally suited for the routine detection of bithionol residues in animal-derived food products with various protein and fat contents.



中文翻译:

通过有效且坚固的萃取方法结合液相色谱-串联质谱法对动物源食品中的联硫酚残留进行分析

本文中,我们开发了一种简单的分析程序,使用改进的快速,简便,廉价,有效,坚固和安全的方法,可定量分析动物源性食品(例如猪肌肉,鸡蛋,牛奶,鳗鱼,比目鱼和虾)中的苯硫酚残留量(QuEChERS)提取方法与液相色谱-电喷雾电离串联质谱(LC-ESI + / MS-MS)结合使用。用0.1%的甲酸在乙腈中的溶液萃取样品,并使用C18吸附剂纯化萃取物。在Waters XBridge™C18反相分析柱上进行分离,使用0.1%的甲酸/乙腈溶液作为流动相。六点矩阵匹配的校准表明线性度好,计算出的测定系数(R 2)≥0.9813。日内和日间回收率(确定为加标水平的1 x和2 x定量限(0.25μg/ kg),介于80.0和94.0%之间,相应的相对标准偏差(RSD)≤8.2% 。发达的实验方案适用于从首尔当地市场购买的不同样品,这些样品中的苯硫酚残留均为阴性。总之,所提出的方法被证明是通用且精确的,非常适合常规检测具有多种蛋白质和脂肪含量的动物源食品中的苯硫酚残留。

更新日期:2017-08-31
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