Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

Bulletin of The Veterinary Institute in Pulawy Pub Date : 2015-09-01 DOI:10.1515/BVIP-2015-0051

A. Gajda, A. Posyniak

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引用次数: 12

Abstract

Abstract A liquid chromatography – tandem mass spectrometry (LC-MS/MS) method for the determination of oxytetracycline (OTC), 4-epi oxytetracycline (4-epi OTC), tetracycline (TC), 4-epi tetracycline (4-epi TC), chlortetracycline (CTC), 4-epi chlortetracycline (4-epi CTC), doxycycline (DC), minocycline (MINO), methacycline (META) and rolitetracycline (ROLI) residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X) reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% – 103.6%. The decision limits were from 109.0 to 119.8 μg/kg and detection capability varied within the range of 122.2 to 137.6 μg/kg, depending on the analyte.

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液相色谱-串联质谱法测定肌肉样品中10种四环素残留

摘要建立了液相色谱-串联质谱(LC-MS/MS)测定肌肉中土霉素(OTC)、4-外皮土霉素(4-epi OTC)、四环素(TC)、4-外皮四环素(4-epi TC)、氯霉素(CTC)、4-外皮四环素(4-epi CTC)、强力霉素(DC)、米诺环素(MINO)、甲氧环素(META)和罗利特环素(ROLI)残留量的方法。该过程包括草酸萃取，然后用三氯乙酸去除蛋白质。进一步在聚合物(Strata X)反相柱上进行固相清理，以获得适合LC-MS/MS分析的提取物。采用c18色谱柱，流动相为0.01%甲酸-乙腈- 0.01%甲酸-水，梯度分离四环素。该方法根据欧盟委员会决议2002/657/EC进行了验证。加样回收率为91.8% ~ 103.6%。决策限为109.0 ~ 119.8 μg/kg，检测能力根据分析物的不同在122.2 ~ 137.6 μg/kg范围内变化。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Bulletin of The Veterinary Institute in Pulawy 农林科学-兽医学

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12-24 weeks