Development of a rapid method for the analysis of trenbolone, nortestosterone, and zeranol in bovine liver using liquid chromatography tandem mass spectrometry

作者：Yunin Maxim A^*; Metalnikov Pavel S; Komarov Alexander A; Panin Alexander N

来源：Analytical and Bioanalytical Chemistry, 2015, 407(15): 4363-4371.

DOI：10.1007/s00216-014-8346-y

• LC-MS/MS
• Bovine liver
• Trenbolone
• Nortestosterone
• Zeranol

A rapid liquid chromatography tandem mass spectrometry method has been developed and validated for the determination of alpha-trenbolone, beta-trenbolone, alpha-nortestosterone, beta-nortestosterone, zeranol, and taleranol in bovine liver. The impact of liquid-liquid extraction with methyl tert-butyl ether and optimized solid phase extraction on silica cartridges significantly reduced effort and time of sample preparation. Electrospray ionization gives a significant signal increase compared with atmospheric pressure chemical ionization and atmospheric pressure photoionization. The HPLC gradient was optimized to separate isobaric analytes and matrix constituents from the hormone molecules. The optimized time and temperature of enzymatic hydrolysis of conjugated trenbolone was 4 h at 52 A degrees C. The method validated in the range of 0.5-30 mu g kg(-1) for alpha-trenbolone, beta-trenbolone, zeranol, taleranol, and 2-30 mu g kg(-1) for alpha-nortestosterone, beta-nortestosterone. Combined uncertainty of measurements was in the range of 4 %-23 %. The matrix effect was negligible (1 %-5 %) for all analytes except of alpha-nortestosterone (19 %). The developed method with changes concerning sample size and hydrolysis was also applied for the analysis of meat, serum, and urine samples.

• 出版日期2015-6