Cho Sang-Hyun, Park Jin-A, Zheng Weijia, Abd El-Aty A M, Kim Seong-Kwan, Choi Jeong-Min, Yi Hee, Cho Soo-Min, Afifi Nehal A, Shim Jae-Han, Chang Byung-Joon, Kim Jin-Suk, Shin Ho-Chul
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea; Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211 Giza, Egypt.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Oct 15;1065-1066:29-34. doi: 10.1016/j.jchromb.2017.09.026. Epub 2017 Sep 19.
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 2ngg, 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.
在本研究中,已开发并验证了一种简单的分析方法,用于使用液相色谱 - 串联质谱法(LC-MS/MS)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醋酸异氟泼尼龙的残留量。使用0.1%的乙酸乙腈溶液与正己烷结合对所有测试基质进行脱蛋白和脱脂处理,目标药物在沃特世Xbridge™ C18分析柱上使用由0.1%乙酸(A)和0.1%乙酸甲醇溶液(B)组成的流动相得到了良好分离。由六点基质匹配校准估计的线性良好,测定系数≥0.9873。盐酸布比卡因和醋酸异氟泼尼龙的定量限(LOQ)分别为1和2ng/g。在三个不同的加标浓度下,盐酸布比卡因的回收率在72.51 - 112.39%范围内,醋酸异氟泼尼龙的回收率在72.58 - 114.56%范围内,相对标准偏差(RSD)<15.14%。实验工作和方法应用的所有样品均从大韩民国首尔的当地市场收集,且均未检测出目标药物呈阳性。总之,一种使用0.1%乙酸乙腈溶液和正己烷然后进行LC-MS/MS的简单方法可以有效地从猪肌肉、牛肉、牛奶、鸡蛋、虾、比目鱼和鳗鱼样品中提取盐酸布比卡因和醋酸异氟泼尼龙。