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宫瘤清片质量标准研究

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目的 建立宫瘤清片的质量标准。方法 采用超高效液相色谱(UPLC)法,色谱柱为Agilent Extend C18 RRHD柱(100 mm × 2。1 mm,1。8 μm),流动相为甲醇-0。4%磷酸水溶液(梯度洗脱),流速为0。3 mL/min,检测波长为220 nm(0~15 min)、250 nm(15~42 min),柱温为30 ℃,进样量为1 μL。将UPLC图谱导入中药色谱指纹图谱相似度评价系统(2012版)建立宫瘤清片的指纹图谱,计算相似度;确定共有峰并指认;并通过聚类分析(CA)、主成分分析(PCA)和偏最小二乘法判别分析(PLS-DA)进行化学模式识别;测定6个指标成分的含量。结果 21批样品的指纹图谱有23个共有峰,指认了6个指标成分,分别为苦杏仁苷、芍药苷、橙皮苷、黄芩苷、甘草酸铵、大黄酚;相似度为0。939~0。996。CA可将样品聚为3类;PCA提取了4个主成分,累计方差贡献率为92。686%;PLS-DA筛选出11个差异化合物。含量测定中,前述6个成分质量浓度在相应范围内与峰面积线性关系良好;精密度、稳定性、重复性试验结果的RSD均小于3。0%;平均加样回收率为91。24%~104。11%,RSD为0。35%~1。95%(n=6)。结论 该制剂中大黄酚为主要差异性成分;建立的方法操作简便、结果准确可靠,可为宫瘤清片的质量控制提供依据。
Study on Quality Standard for Gongliuqing Tablets
Objective To establish the quality standard of Gongliuqing Tablets.Methods The ultra-high-performance liquid chromatography(UPLC)method was adopted;the chromatographic column was the Agilent Extend C18 RRHD column(100 mm × 2.1 mm,1.8 μm),the mobile phase was methanol-0.4%phosphoric acid aqueous solution(gradient elution),the flow rate was 0.3 mL/min,the detection wavelengths were 220 nm(0-15 min)and 250 nm(15-42 min),the column temperature was 30℃,and the injection volume was 1 μL.The UPLC chromatograms were imported into the similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine(version 2012)to establish the fingerprint of Gongliuqing Tablets,the similarity was calculated,the common peaks were marked and identified;the chemical pattern recognition was performed through cluster analysis(CA),principal component analysis(PC A),and partial least squares-discriminant analysis(PLS-DA);and the contents of six indicator components were determined.Results There were 23 common peaks in the fingerprint of 21 batches of samples,and six indicator components were identified,namely amygdalin,paeoniflorin,hesperidin,baicalin,ammonium glycyrrhizinate and chrysophanol;the similarity was in the range of 0.939 to 0.996.The samples were grouped into three categories by the CA;four principal components were extracted by the PCA,with a cumulative variance contribution rate of 92.686%;11 differential compounds were screened by the PLS-DA.In the content determination,the mass concentration of the above six components had a good linear relationship with the peak area within the corresponding range;the RSDs of precision,stability and repeatability tests were lower than 3.0%;the recovery rates of the above six components were in the range of 91.24%to 104.11%,with the RSDs of 0.35%to 1.95%(n=6).Conclusion Chrysophanol was the main differential component in this preparation.The established method is easy,accurate and reliable,which can provide a basis for quality control of Gongliuqing Tablets.

Gongliuqing TabletsUPLCfingerprintchemical pattern recognitionquality control

赵文艳、朱法根、刘雪、王玲玲、李超

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济川药业集团有限公司,江苏 泰州 225441

宫瘤清片 超高效液相色谱法 指纹图谱 化学模式识别 质量控制

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(24)