Bian Kui, Lin Tao, Liu Min, Yang Jianwen, Wang Zongnan, He Limin
Se Pu. 2014 Feb;32(2):162-8. doi: 10.3724/sp.j.1123.2013.08031.
A gas chromatography-mass spectrometry (GC-MS) method was established for the determination of the residues of three beta-agonists (clenbuterol, salbutamol and ractopamine) in pig edible tissues. The matrix effects (MEs) in the analysis of the three compounds with the developed method were determined. The influences of matrix state and its weight on MEs were evaluated statistically. The analytes in pig liver and muscle and their corresponding freeze-dried powders were derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide. Then the derivatives were determined in selected ion monitoring mode and the intensities of MEs of the three beta-agonists were obtained. Significant matrix enhancement was observed for the three analytes, and especially, the ME of ractopamine was more than 1000%. The results of analysis of variance (ANOVA) demonstrated that MEs were significantly different for the three analytes in two matrices among different matrix weights (P < 0.05), and MEs of the three analytes increased from 1 g to 5 g with the increase of matrix weight. MEs for the three analytes were not significantly different between fresh pig tissues and its freeze-dried powder matrices (P > 0.05), indicating that the freeze-dried powder matrices might be used to conveniently prepare the matrix-matched calibration solution, which could efficiently compensate the MEs of the beta-agonists in GC-MS analysis.
建立了气相色谱-质谱联用(GC-MS)法测定猪可食组织中三种β-激动剂(克伦特罗、沙丁胺醇和莱克多巴胺)的残留量。采用所建立的方法测定了三种化合物分析中的基质效应(MEs)。对基质状态及其重量对基质效应的影响进行了统计学评估。用N,O-双(三甲基硅基)三氟乙酰胺对猪肝和肌肉及其相应的冻干粉中的分析物进行衍生化。然后在选择离子监测模式下测定衍生物,并获得三种β-激动剂的基质效应强度。观察到三种分析物均有显著的基质增强,尤其是莱克多巴胺的基质效应超过1000%。方差分析(ANOVA)结果表明,不同基质重量下两种基质中三种分析物的基质效应存在显著差异(P<0.05),且三种分析物的基质效应随基质重量从1 g增加到5 g而增加。三种分析物在新鲜猪组织及其冻干粉基质中的基质效应无显著差异(P>0.05),表明冻干粉基质可方便地制备基质匹配校准溶液,能有效补偿GC-MS分析中β-激动剂的基质效应。