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Quantification of bupivacaine hydrochloride and isoflupredone acetate residues in porcine muscle, beef, milk, egg, shrimp, flatfish, and eel using a simplified extraction method coupled with liquid chromatography–triple quadrupole tandem mass spectrometry
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2017-09-19 , DOI: 10.1016/j.jchromb.2017.09.026
Sang-Hyun Cho , Jin-A Park , Weijia Zheng , A.M. Abd El-Aty , Seong-Kwan Kim , Jeong-Min Choi , Hee Yi , Soo-Min Cho , Nehal A. Afifi , Jae-Han Shim , Byung-Joon Chang , Jin-Suk Kim , Ho-Chul Shin

In this study, a simple analytical approach has been developed and validated for the determination of bupivacaine hydrochloride and isoflupredone acetate residues in porcine muscle, beef, milk, egg, shrimp, flatfish, and eel using liquid chromatography-tandem mass spectrometry (LC–MS/MS). A 0.1% solution of acetic acid in acetonitrile combined with n-hexane was used for deproteinization and defatting of all tested matrices and the target drugs were well separated on a Waters Xbridge™ C18 analytical column using a mobile phase consisting of 0.1% acetic acid (A) and 0.1% solution of acetic acid in methanol (B). The linearity estimated from six-point matrix-matched calibrations was good, with coefficients of determination ≥0.9873. The limits of quantification (LOQs) for bupivacaine hydrochloride and isoflupredone acetate were 1 and 2 ng g−1, respectively. Recovery percentages in the ranges of 72.51–112.39% (bupivacaine hydrochloride) and 72.58–114.56% (isoflupredone acetate) were obtained from three different fortification concentrations with relative standard deviations (RSDs) of <15.14%. All samples for the experimental work and method application were collected from the local markets in Seoul, Republic of Korea, and none of them tested positive for the target drugs. In conclusion, a simple method using a 0.1% solution of acetic acid in acetonitrile and n-hexane followed by LC–MS/MS could effectively extract bupivacaine hydrochloride and isoflupredone acetate from porcine muscle, beef, milk, egg, shrimp, flatfish, and eel samples.



中文翻译:

简化提取方法结合液相色谱-三重串联四极杆串联质谱法定量分析猪肌肉,牛肉,牛奶,鸡蛋,虾,比目鱼和鳗鱼中盐酸布比卡因和乙酸异氟泼酮的残留量

在这项研究中,已开发出一种简单的分析方法,并已通过液相色谱-串联质谱法(LC-MS)用于测定猪肌肉,牛肉,牛奶,鸡蛋,虾,比目鱼和鳗鱼中盐酸布比卡因和乙酸异氟泼酮残留量的测定。 /多发性硬化症)。0.1%的乙酸在乙腈中的溶液与n正己烷用于所有测试基质的脱蛋白和脱脂,目标药物在Waters Xbridge™C18分析柱上使用0.1%乙酸(A)和0.1%乙酸的甲醇溶液( B)。根据六点矩阵匹配的校准估计的线性良好,测定系数≥0.9873。盐酸布比卡因和乙酸异氟泼酮的定量限(LOQs)为1和2 ng g -1, 分别。从三种不同的设防浓度得到的回收率分别为72.51–112.39%(盐酸布比卡因)和72.58–114.56%(乙酸异氟泼酮),相对标准偏差(RSD)为<15.14%。所有用于实验工作和方法应用的样品均从大韩民国首尔的当地市场采集,且均未检测到目标药物呈阳性。总之,一个简单的方法,使用在乙腈中的乙酸的0.1%溶液和Ñ己烷,随后通过LC-MS / MS可以有效地从猪的肌肉,牛肉,牛奶,鸡蛋,虾,比目鱼提取盐酸布比卡因和异氟泼尼龙醋酸酯,和鳗鱼样品。

更新日期:2017-09-19
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