基于多指标含量测定及HPLC特征图谱结合化学计量学的解郁安神颗粒质量综合评价  

Comprehensive quality evaluation of Jieyu Anshen granules based on multi-indicator content determination and HPLC characteristic chromatogram combined with chemometrics

作　　者：燕霞 朱韬 何颂华 罗轶 YAN Xia;ZHU Tao;HE Song-hua;LUO Yi(Guangxi Institute for Food and Drug Control NMPA Key Laboratory for Quality Monitpring and Evaluation of Traditional Chinese Medicine,Chinese Materia Medica,Nanning 530021,China)

机构地区：[1]广西壮族自治区药品检验研究院、国家药品监督管理局中药材质量监测与评价重点实验室,南宁530021

出　　处：《药物分析杂志》2024年第9期1567-1577,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：2023国家药品抽检品种项目(序号26)。

摘　　要：目的:建立解郁安神颗粒的多组分含量测定及特征图谱方法与化学计量学结合,对解郁安神颗粒质量进行整体评价。方法:采用CAPCELL PAK MGⅡC_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温30℃,检测波长在237 nm(栀子苷、甘草苷、甘草酸铵)和335 nm(斯皮诺素及3,6’-二芥子酰基蔗糖)5个成分进行含量测定并进行方法学验证。基于多组分含量测定方法,建立样品的特征图谱,并通过化学计量学对样品进行分析评价,找出影响样品质量的主要因素。结果:建立了解郁安神颗粒的多组分含量测定方法,5个成分在各自范围内线性关系良好,回收率在95.6%~100.0%,对145批次样品进行测定,不合格样品共54批,总不合格率为37.2%;建立了解郁安神颗粒的特征图谱,标定了12个特征峰分别归属于6味药材,通过化学计量学软件分析,10个厂家样品质量存在一定差异,炒栀子与炙甘草质量的优劣是影响样品质量的关键因素。结论:建立的解郁安神颗粒多组分含量测定方法及特征图谱方法便捷可靠,可用于解郁安神颗粒品质的综合评价。Objective:To establish a multi-component content determination and characteristic chromatogram method for Jieyu Anshen granules,combined with chemometrics,to comprehensively evaluate the quality of Jieyu Anshen granules.Methods:The separation was performed on a CAPCELL PAK MGⅡC_(18)(250 mm×4.6 mm,5μm)column using acetonitrile(A)and 0.1%phosphoric acid aqueous solution(B)as the mobile phases with gradient elution at a flow rate of 1.0 mL·min^(-1).The column temperature was 30℃and the detection wavelengths were set at 237 nm and 335 nm.The analysis method was validated.Based on the multi-component content determination method,characteristic chromatogram was established.The samples were analyzed and evaluated through chemometrics to identify the main factors affecting their quality.Results:A multi-component content determination method was established for Jieyu Anshen granules.The five components had good linear relationships within their respective ranges,with recovery rates ranging from 95.6%to 100.0%.And 145 batches of samples were tested,and a total of 54 batches were found to be unqualified,with a total unqualified rate of 37.2%.Establishing a characteristic chromatogram of Anshen granules,12 characteristic peaks were attributed to 6 medicinal herbs.Through chemometric analysis,it was found that there were certain differences in the quality of samples from 10 manufacturers.The quality of fried gardenia and stir-baked licorice was the key factor.Conclusion:The established multi-component content determination method and characteristic chromatogram method for Jieyu Anshen granules are convenient and reliable,and can be used for comprehensive evaluation of the quality of Jieyu Anshen granules.

关 键 词：解郁安神颗粒 含量测定 栀子苷 甘草苷 甘草酸铵 斯皮诺素 3 6’-二芥子酰基蔗糖 特征图谱 质量评价 

分 类 号：R917[医药卫生—药物分析学]