小儿清热宁颗粒HPLC指纹图谱研究及其多指标成分定量分析  

Fingerprint and Multi-component Determination of Xiaoer Qingrening Granules by HPLC

作　　者：唐春梅 刘申平[2] Tang Chunmei;Liu Shenping(Department of Pharmacy,Zigong First People's Hospital,Sichun Zigong 646000,China;Department of cardiothoracic surgery,Zigong First People's Hospital,Sichun Zigong 646000,China)

机构地区：[1]自贡市第一人民医院药剂科,四川自贡646000 [2]自贡市第一人民医院胸心外科,四川自贡646000

出　　处：《中国药师》2021年第6期1146-1152,共7页China Pharmacist

摘　　要：目的:建立小儿清热宁颗粒的HPLC指纹图谱,并进行多成分定量分析,用于评价小儿清热宁颗粒的质量。方法:采用Agilent SB-C18色谱柱(250 mm×4.6 mm,5μm)进行检测,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱;流速为1.0 ml·min^(-1);检测波长为254,327 nm;柱温为35℃。通过相似度评价结合聚类分析对小儿清热宁颗粒指纹图谱进行质量评价,并对指认的8个指标成分进行定量分析。结果:在特征指纹图谱研究中,以黄芩苷为参照峰,共标定29个共有峰,12批小儿清热宁颗粒与共有模式对照图谱之间有良好的相似性,相似度均在0.90以上;在建立的色谱条件下,8个成分分离度良好,方法精密度和重复性RSD均小于2.0%,供试品溶液在48 h内稳定,各成分具有良好的线性关系和较宽线性范围,平均加样回收率在98.27%~104.55%之间,RSD在1.04%~2.25%之间。12批样品中(R,S)-告依春、绿原酸、黄芩苷、汉黄芩苷、柴胡皂苷a、柴胡皂苷d、黄芩素和汉黄芩素含量范围分别为0.0310~0.0660mg·g^(-1)、0.3390~0.6740 mg·g^(-1)、1.5240~2.9540 mg·g^(-1)、0.0580~0.2100 mg·g^(-1)、0.3440~0.5460 mg·g^(-1)、0.6950~1.1140 mg·g^(-1)、0.1010~0.1970 mg·g^(-1)、0.1220~0.2110 mg·g^(-1)。通过聚类分析,12批供试品聚成3类。结论:所建立的小儿清热宁颗粒HPLC指纹图谱和含量测定方法灵敏度高,专属性强、可以用于该制剂的质量控制。Objective:To establish fingerprint and multi-component determination method for Xiaoer Qingrening granules to provide reference for quality evaluation.Methods:The analysis was performed on an Agilent SB-C18column(250 mm×4.6 mm,5μm),and the mobile phase consisted of acetonitrile-0.1% phosphoric acid with gradient elution.The detection wavelengths were set at 254 nm and 327 nm at the flow rate of 1.0 ml·min^(-1).The column temperature was set at 35℃.Similarity evaluation combined with cluster analysis(CA)was used to evaluate the fingerprint of Xiaoer Qingrening granules,and eight markers were quantified.Results:Totally29 common peaks were recognized with baicalin as the reference peak.There were good similarities between the standard characteristic chromatogram and each characteristic chromatogram of 12 samples with the similarities over 0.90.The 8 compounds were well separated under the determined chromatographic conditions.The RSDs of precision and repeatability experiments were all less than 2.0%.And the sample solution was stable within 48 h.All the compounds had good linearity and wide linear ranges.The average recoveries ranged from 98.27% to 104.55% with the RSDs of 1.04%-2.25%.The content range of(R,S)-goitrin,chlorogenic acid,baicalin,wogonoside,saikosaponin a,saikosaponin d,baicalein and wogonin was 0.0310-0.0660 mg·g^(-1),0.3390-0.6740 mg·g^(-1),1.5240-2.9540 mg·g^(-1),0.0580-0.2100 mg·g^(-1),0.3440-0.5460 mg·g^(-1),0.6950-1.1140 mg·g^(-1),0.1010-0.1970 mg·g^(-1) and 0.1220-0.2110 mg·g^(-1),respectively.All 12 batches of samples could be classified into three clusters by CA.Conclusion:The established method has high sensitivity and specificity,and can be used for the quality control of Xiaoer Qingrening granules.

关 键 词：小儿清热宁颗粒 高效液相色谱法 指纹图谱 相似度分析 聚类分析 

分 类 号：TQ460.72[医药卫生—药物分析学]