UPLC-MSMS法测定大黄碳酸氢钠片和复方龙胆碳酸氢钠片中土大黄苷的含量  

Quantitative Determination of Rhaponticin in Rhubarb Sodium Bicarbonate Tablets,Compound Gentian and Sodium Bicarbonate Tablets by UPLC-MS/MS

作　　者：胡珀[1] 吴旭[1] 王蓓蓓[1] 金鹏[1] HU Po;WU Xu;WANG Bei-bei;JIN Peng(Huai′an Institute for Food and Drug Control,Jiangsu Huai′an 223001,China)

机构地区：[1]淮安市食品药品检验所,江苏淮安223001

出　　处：《中国药物评价》2020年第5期362-365,共4页Chinese Journal of Drug Evaluation

摘　　要：目的:建立大黄碳酸氢钠片和复方龙胆碳酸氢钠片中伪品大黄指标性成分土大黄苷含量的定量测定方法。方法:本次的样品共11批次,包括7批大黄碳酸氢钠片,4批复方龙胆碳酸氢钠片,采用超高效液相色谱-质谱联用法(UPLC-MS/MS)对土大黄苷含量进行测定。结果:方法学考察结果显示,土大黄苷质量浓度在0.5~500 ng·mL^-1范围内与峰面积呈良好的线性关系(r=0.9992);检出限、定量限分别为5、15 ng·g^-1;精密度、重复性、稳定性试验RSD均小于1%;大黄碳酸氢钠片平均加样回收率为95.16%(RSD=1.07%,n=6),复方龙胆碳酸氢钠片平均加样回收率为96.13%(RSD=1.46%,n=6)。4批样品中土大黄苷含量为7.6~3392.1μg·g^-1。结论:建立UPLC-MS/MS法操作简便、灵敏、可靠,可用于大黄碳酸氢钠片和复方龙胆碳酸氢钠片中土大黄苷的定量测定。Objective:To establish a method for quantitative determination of indicative composition rhaponiticin from counterfeit Rheum palmatum in rhubarb sodium bicarbonate tablets,compound gentian and sodium bicarbonate tablets.Methods:7 batches of Rhubarb Sodium Bicarbonate Tablets,4 batches of compound gentian and sodium bicarbonate tablets were collected,totaling 11 batches.The content of rhaponiticin was determined by UPLC-MS/MS method.Results:UPLC-MS/MS methodology investigation showed that the linear range of rhaponiticin was 0.5-500 ng·mL^-1(r=0.9992).The detection limit and quantitative limit were 5,15 ng·g^-1.RSDs of precision,reproducibility and stability tests were all lower than 1%.Average recovery of rhubarb sodium bicarbonate tablets was 95.16%(RSD=1.07%,n=6),average recovery of compound gentian and sodium bicarbonate tablets was 96.13%(RSD=1.46%,n=6).The contents of rhaponiticin in 4 batches of samples were 7.6~3392.1μg·g^-1.Conclusion:UPLC-MS/MS for content determination is simple,sensitive and reliable,and can be used for quantitative determination of rhaponiticin in Rhubarb sodium bicarbonate tablets,compound gentian and sodium bicarbonate tablets.

关 键 词：大黄碳酸氢钠片 复方龙胆碳酸氢钠片 土大黄苷 超高效液相色谱-质谱联用法 

分 类 号：R917[医药卫生—药物分析学]