氘代内标法测定药用牡蛎中的三苯甲烷类染料.pdf

氘代内标法测定药用牡蛎中的三苯甲烷类染料 1 1* 2 1 甘盛 ，施晓光 ，韩婷 ，吴超权 (1.广西壮族自治区食品药品检验所，南宁530021；2.河北联合大学基础药学院药理教研室，河北 唐山 063009) 摘要：目的 建立用液相-质谱串联联用仪，使用氘代内标测定药用牡蛎中三苯甲烷类染料残留的方法，以提高牡蛎药材 的安全性。方法 样品溶液加入氘代混合内标，中性氧化铝固相萃取小柱净化后过WAX 小柱分离，用乙腈对WAX 小柱 进行洗脱后吹干，残余物溶于50%乙腈水溶液，用液质串联联用仪测定，梯度洗脱，流动相为乙腈-5 mmol·L1 乙酸铵溶 液。结果 各分子在0.5~10 μg·kg1 内线性关系良好，平均回收率为90.5%~102.6% ，定量限为0.054 3~0.29 78 μg·kg1。 结论 此方法灵敏准确，专属性强，干扰少，重复性佳，对检测牡蛎药材中的三苯甲烷类染料残留极具参考价值。 关键词：药用牡蛎；氘代内标；孔雀石绿；隐色孔雀石绿；结晶紫；隐色结晶紫 中图分类号：R931.77 文献标志码：B 文章编号：1007-7693(2012)09-0836-05 Quantitative Determination of Triphenylmethane Dyes in Medicinal Oyster by Deuterated Internal Standard Method 1 1* 2 1 GAN Sheng , SHI Xiaoguang , HAN Ting , WU Chaoquan (1.Guangxi Institute for Food and Drug Control, Nanning 530021, China; 2.Didactic and Research Section of Pharmacology, College of Fundamental Pharmacy, Hebei United University, Tangshan 063009, China) ABSTRACT: OBJECTIVE To approach the determination of the residues of deuterated internal standard in medicinal oyster by LC-MS/MS with deuterated internal standard to improve the safety of medicinal oyster materials. METHODS A mixture of deuterated internal standard was added to the samples, purified by acidic alumina cartridges and then isolated through acidic alumina cartridges. Elute the alumina cartridges with acetonitrile, and the residue was tested by LC-MS/MS, with the gradient of mobile phase composed of acetonitrile and 5 mmol·L1 ammonium acetate solution. RESULTS All molecules in samples were in good linear of 0.510 μg·kg1, with a mean recovery at 90.5%~102.6%, and the instrumental limit of quantitative detection was 0.054 30.297 8 μg·kg1. CONCLUSION The method is proved to be sensitive and accurate, repeatable and specific with little interference, extremely consultable for inspection for residues of triphenylmethane dyes