Xu Jin-Zhong, Ding Tao, Wu Bin, Yang Wen-Quan, Zhang Xiao-Yan, Liu Yan, Shen Chong-Yu, Jiang Yuan
Animal, Plant and Food Inspection Center, Jiangsu Entry-Exit Inspection and Quarantine Bureau, National Bee-Product Reference Laboratory, Nanjing, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Jun 1;868(1-2):42-8. doi: 10.1016/j.jchromb.2008.04.027. Epub 2008 Apr 25.
A confirmatory method coupling liquid chromatography with tandem mass spectrometry (LC/MS/MS) was developed to determine the concentration of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC) and doxycycline (DC), which make up the tetracycline (TC) groups present in royal jelly. Sample preparation included deproteination, control of pH, extraction and clean-up on a solid-phase extraction (SPE) cartridge. The analyses were achieved by LC/MS/MS in selected reaction monitoring mode (SRM). The overall recovery of fortified royal jelly at the levels of 5.0, 10.0 and 40.0 microg/kg ranged from 62% to 115%, and the coefficients of variation ranged from 3.4% to 16.3% (n=6). The detection limits for TCs were under 1.0 microg/kg. The transformation between the TCs and its epimers (EpiTCs) was studied in standard solution and during the sample preparation process. This method can be used for the detection of tetracycline residues in royal jelly.
建立了一种液相色谱-串联质谱联用(LC/MS/MS)的确证方法,用于测定蜂王浆中组成四环素(TC)类的土霉素(OTC)、四环素(TC)、金霉素(CTC)和强力霉素(DC)的浓度。样品制备包括脱蛋白、pH值控制、提取以及在固相萃取(SPE)柱上进行净化。分析通过LC/MS/MS在选择反应监测模式(SRM)下完成。在5.0、10.0和40.0微克/千克水平下加标蜂王浆的总回收率在62%至115%之间,变异系数在3.4%至16.3%之间(n = 6)。四环素类的检测限低于1.0微克/千克。在标准溶液和样品制备过程中研究了四环素类及其差向异构体(EpiTCs)之间的转化。该方法可用于检测蜂王浆中的四环素残留。