大黄通便片中非法成分土大黄苷的定性筛查和定量测定研究  

Study on Qualitative Screening and Quantitative Determination of Rhaponticin in Dahuang Tongbian Tablets

作　　者：肖小武 周志强 洪挺 杨毅生 万林春 XIAO Xiao-wu;ZHOU Zhi-qiang;HONG Ting;YANG Yi-sheng;WAN Lin-chun(Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality,NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine,Jiangxi Institute For Drug Control,Jiangxi Nanchang 330029,China)

机构地区：[1]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,江西南昌330029

出　　处：《中国药物评价》2024年第4期289-295,共7页Chinese Journal of Drug Evaluation

基　　金：江西省重大研发项目“江西省中药饮片炮制规范及我省道地药材品质提升研究(2023BBG7001)”。

摘　　要：目的:建立大黄通便片中土大黄苷的定性筛查和定量测定方法。方法:采用薄层色谱(TLC)法初筛,高效液相色谱(HPLC)法定量测定及超高效液相色谱-质谱联用(UHPLC-MS)法定性确证。结果:TLC法检测结果显示专属性强,耐用性好。HPLC法方法学考察结果显示:土大黄苷质量浓度在2.59~259.6μg·mL^(-1)范围内呈良好的线性关系(R^(2)=0.9999);精密度、重复性、稳定性试验RSD均小于2.0%;平均加样回收率为97.89%(RSD=0.61%)。UHPLC-MS/MS法确证结果与TLC、HPLC法结果一致,阳性检出样品与土大黄苷对照品呈现同一保留时间的提取离子对(421.1→258.9,421.1→199.0)。结论:该方法灵敏、准确,可作为大黄通便片中非法成分土大黄苷的检查方法。Objective:To establish a method for the qualitative screening and quantitative determination of rhein in Dahuang Tongbian tablets.Methods:TLC was used for preliminary screening,HPLC was used for quantitative determination,and UHPLC-MS was used for qualitative confirmation.Results:TLC test results showed strong specificity and good durability.HPLC results showed that the mass concentration of rhein showed a good linear relationship in the range of 2.59~259.6μg·mL^(-1)(R^(2)=0.9999).RSDS of precision,repeatability and stability tests were all less than 2.0%.The average recovery was 97.89%(RSD=0.61%).The confirmed results of UHPLC-MS/MS were consistent with TLC and HPLC,and the extracted ion pairs with the same retention time of the positive samples and the control products of rhein(421.1→258.9,421.1→199.0).Conclusion:The method is sensitive and accurate,and can be used as a method for the detection of illegal components of rhein in Dahuang Tongbian tablets.

关 键 词：大黄通便片 土大黄苷 薄层色谱(TLC) 高效液相色谱(HPLC) 超高效液相色谱-质谱联用(UHPLC-MS/MS) 

分 类 号：R284.2[医药卫生—中药学]