首页|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

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

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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(R2=0.999 9);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.
Study on Qualitative Screening and Quantitative Determination of Rhaponticin in Dahuang Tongbian Tablets
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 con-centration of rhein showed a good linear relationship in the range of 2.59～259.6 μg·mL-1(R2=0.999 9).RSDS of precision,repeat-ability and stability tests were all less than 2.0％.The average recovery was 97.89％(RSD=0.61％).The confirmed results of UH-PLC-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.

Dahuang Tongbian TabletsRhaponticinThin Layer Chromatography(TLC)High Performance Liquid Chromatography(HPLC)Ultra-High-Performance Liquid Chromatography Mass Spectrometer(UHPLC-MS/MS)

肖小武、周志强、洪挺、杨毅生、万林春

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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

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)

2024

中国药物评价
国家食品药品监督管理局信息中心

中国药物评价

影响因子：1.09
ISSN：2095-3593
年,卷(期)：2024.41(4)