首页|基于UHPLC多成分测定与主成分分析的金藤清痹颗粒质量评价

基于UHPLC多成分测定与主成分分析的金藤清痹颗粒质量评价

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目的:建立同时测定金藤清痹颗粒中青藤碱、新绿原酸、木兰花碱、隐绿原酸、绿原酸、异绿原酸B、异绿原酸A、异绿原酸C、哈巴俄苷、藁本内酯和甘草酸铵11个成分含量的UHPLC法,并结合主成分分析对制剂进行质量评价.方法:采用UHPLC波长切换法,色谱柱为Waters XSelect ® CSH C18柱(150 mm ×4.6 mm,2.5 µm),以甲醇-乙腈(1∶1)为流动相A,0.2%磷酸水溶液为流动相B,梯度洗脱,流速1.0 mL·min-1,柱温25℃,检测波长218 nm(0~17 min时,检测青藤碱)、326 nm(17~25 min和34~98 min时,检测新绿原酸、隐绿原酸、绿原酸和异绿原酸A、异绿原酸B、异绿原酸C)、263 nm(25~34 min和98~125 min时,检测木兰花碱、哈巴俄苷、藁本内酯、甘草酸铵).利用SPSS27.0软件对20批金藤清痹颗粒中成分含量进行多元统计分析.结果:青藤碱、新绿原酸、木兰花碱、隐绿原酸、绿原酸、异绿原酸B、异绿原酸A、异绿原酸C、哈巴俄苷、藁本内酯和甘草酸铵11个成分的质量浓度分别在 14.36~143.61 µg·mL-1(r=0.999 9)、7.71~77.15 μg·mL-1(r=0.999 8)、9.18~91.83 μg·mL-1(r=0.999 7)、10.71~107.07 μg·mL-1(r=0.999 8)、12.88~128.80 μg·mL-1(r=0.999 8)、5.20~51.95 μg·mL-1(r=0.999 7)、5.18~51.84μg·mL-1(r=0.999 8)、5.40~53.95 μg·mL-1(r=0.999 8)、2.62~26.16 μg·mL-1(r=0.999 9)、6.31~63.06 μg·mL-1(r=0.999 9)和 11.13~111.26 μg·mL-1(r=0.997 6)范围内与峰面积的线性关系良好;平均加样回收率(n=6)分别为98.3%、98.3%、98.5%、98.9%、99.2%、101.0%、98.1%、97.1%、96.8%、98.0%和 98.7%,RSD 均小于 3.0%.20 批金藤清痹颗粒样品中,上述青藤碱等11个成分的含量测定结果(n=6)依次为2.206~2.704、1.071~1.403、2.096~2.487、1.321~1.724、2.241~2.612、0.605~0.749、0.363~0.412、0.835~1.020、0.151~0.191、0.791~1.188和1.008~1.363 mg·g-1.主成分分析结果显示,连续生产的金藤清痹颗粒批次间质量差异较小,且以样品S1、S5和S7的综合质量相对更好.结论:建立的UHPLC多指标成分含量测定方法简便、准确、稳定,结合主成分分析,可全面地评价金藤清痹颗粒的产品质量.
Quality evaluation of Jinteng Qingbi granules based on UHPLC multi-index component determination and principal component analysis
Objective:To establish a UHPLC method for simultaneously determining sinomenine,neochlorogenic acid,magnolflorine,cryptochlorogenic acid,chlorogenic acid,isochlorogenic acid B,isochlorogenic acid A,isochlorogenic acid C,harpagoside,ligustilide and ammonium glycyrrhizate in Jinteng Qingbi granules,and evalu-ate the quality of Jinteng Qingbi granules combined with principal component analysis.Methods:UHPLC wave-length switching method was employed in the study.The chromatographic separation was performed on a Waters XSelect ® CSH C18 column(150 mm ×4.6 mm,2.5 μm)using methanol-acetonitrile(1∶1)as mobile phase A and 0.2%phosphoric acid aqueous solution as mobile phase B in a gradient mode at 25 ℃.The flow rate was 1.0 mL·min-1,and the UV detection wavelength was chosen at 218 nm for sinomenine during 0-17 min,326 nm for neochlorogenic acid,cryptochlorogenic acid,chlorogenic acid,isochlorogenic acid B,isochlorogenic acid A and isochlorogenic acid C during 17-25 min and 34-98nm,263 nm for magnolflorine,harpagoside,ligustil-ide and ammonium glycyrrhizate during 25-34 min and 98-125nm,respectively.Furthermore,multiple statisti-cal analysis was conducted on the contents of 11 components in 20 batches of Jinteng Qingbi granules using SPSS27.0 software.Resluts:Satisfactory linearities of sinomenine,neochlorogenic acid,magnolflorine,crypto-chlorogenic acid,chlorogenic acid,isochlorogenic acid B,isochlorogenic acid A,isochlorogenic acid C,harpago-side,ligustilide and ammonium glycyrrhizate were in the ranges of 14.36-143.61 μg·mL-1(r=0.999 9),7.71-77.15 μg·mL-1(r=0.999 8),9.18-91.83 μg·mL-1(r=0.999 7),10.71-107.07 μg·mL-1(r=0.999 8),12.88-128.80 μg·mL-1(r=0.999 8),5.20-51.95 μg·mL-1(r=0.999 7),5.18-51.84 μg·mL-1(r=0.999 8),5.40-53.95 μg·mL-1(r=0.999 8),2.62-26.16 μg·mL-1(r=0.999 9),6.31-63.06 μg·mL-1(r=0.999 9)and 11.13-111.26 μg·mL-1(r=0.997 6),respec-tively.The average recoveries(n=6)were 98.3%,98.3%,98.5%,98.9%,99.2%,101.0%,98.1%,97.1%,96.8%,98.0%and 98.7%,respectively,with RSDs less than 3.0%.The contents ranges of sinome-nine and other 10 components of 20 batches of Jinteng Qingbi granules samples were 2.206-2.704,1.071-1.403,2.096-2.487,1.321-1.724,2.241-2.612,0.605-0.749,0.363-0.412,0.835-1.020,0.151-0.191,0.791-1.188 and 1.008-1.363 mg·g-1,respectively.The results of principal component a-nalysis showed that the quality differences between batches of continuously produced Jinteng Qingbi granules were relatively smaller,and the comprehensive quality of samples S1,S5 and S7 was relatively better.Conclusion:The established UHPLC method of multi-index component determination is simple,accurate and stable.Combined with principal component analysis,it can be used for quality evaluation of Jinteng Qingbi granules comprehensively.

Jinteng Qingbi granulesUHPLCwavelength switchingcontent determinationprincipal component analysisquality evaluation

邓丽华、许克宁、袁晓梅、丁兵、王丽苹、徐丽、杨本官、刘源慧、范建伟

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鲁南制药集团股份有限公司经方与现代中药融合创新全国重点实验室,临沂 276006

鲁南厚普制药有限公司中药制药共性技术山东省工程研究中心,临沂 276006

金藤清痹颗粒 超高效液相色谱 波长切换 含量测定 主成分分析 质量评价

山东省重点研发计划(重大科技创新工程)山东省新旧动能转换重大产业攻关项目

2021CXGC010508鲁动能办[2021]23号

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(3)
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