摘要
目的建立黄芪桂枝五物汤的高效液相色谱(HPLC)指纹图谱及多指标成分含量测定方法。方法采用HPLC法,色谱柱为Waters SunFire^(TM)C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%甲酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长为254 nm,柱温为40℃,进样量为10μL。以桂皮醛峰为参照,测定10批样品的HPLC指纹图谱,采用中药色谱指纹图谱相似度评价系统(2012A版)进行相似度评价,并对共有峰进行鉴定和药材归属。在上述色谱条件下测定芍药内酯苷、芍药苷、毛蕊异黄酮苷、桂皮酸、桂皮醛的含量。结果10批样品共有17个共有峰,相似度均大于0.990;经验证,10批样品HPLC图谱与对照指纹图谱一致性较好。上述5种成分质量浓度分别在19.0~171.0μg/mL、61.6~555.0μg/mL、8.3~75.0μg/mL、18.0~162.0μg/mL、28.4~255.9μg/mL范围内与峰面积线性关系良好;检测限为0.1~1.2μg/mL,定量限为0.3~4.9μg/mL;精密度、稳定性、重复性试验结果的RSD均小于3.0%;平均加样回收率分别为99.31%,98.93%,100.89%,98.83%,100.85%,RSD分别为0.25%,0.30%,0.60%,1.99%,0.74%(n=6)。结论该方法操作简便,稳定可行,重复性好,可用于黄芪桂枝五物汤的质量控制。
Objective To establish a high-performance liquid chromatography(HPLC)fingerprint of Huangqi Guizhi Decoction and a content determination method of multi-indicator components.Methods The HPLC method was adopted.The chromatographic column was the Waters SunFire^(TM) C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.1%formic acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 254 nm,the column temperature was 40℃,and the injection volume was 10μL.The HPLC fingerprint of 10 batches of samples was established with cinnamaldehyde peak as a reference.The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(2012A Version)was used for similarity evaluation.The common peaks were identified,and the medicinal herb attribution analysis was conducted.The contents of albiflorin,paeoniflorin,calycosin-7-O-β-D-glucoside,cinnamic acid and cinnamaldehyde were determined by the above chromatographic conditions.Results A total of 17 common peaks in 10 batches of samples were identified,with the similarity greater than 0.990.The verification test showed that the HPLC fingerprint of 10 batches of samples was consistent with the reference fingerprint.The linear ranges of albiflorin,paeoniflorin,calycosin-7-O-β-D-glucoside,cinnamic acid and cinnamaldehyde were 19.0-171.0μg/mL,61.6-555.0μg/mL,8.3-75.0μg/mL,18.0-162.0μg/mL and 28.4-255.9μg/mL,respectively.The limit of detection was in the range of 0.1-1.2μg/mL,and the limit of quantitation was in the range of 0.3-4.9μg/mL.The RSDs of precision,stability and repeatability tests were all lower than 3.0%.The average recovery rates of the above five components were 99.31%,98.93%,100.89%,98.83%,100.85%with the RSD of 0.25%,0.30%,0.60%,1.99%,0.74%respectively(n=6).Conclusion The method is sample,stable,feasible and repeatable,which can be used for quality control of Huangqi Guizhi Wuwu Decoction.
作者
张顺宵
陈月
苟小军
ZHANG Shunxiao;CHEN Yue;GOU Xiaojun(Endocrine and Metabolic Disease Center,Baoshan District Hospital of Integrated Traditional Chinese Medicine and Western Medicine,Shanghai,China 201999)
出处
《中国药业》
CAS
2024年第14期70-75,共6页
China Pharmaceuticals
基金
上海市卫生和计划生育委员会科研课题[20184Y0092]
上海市宝山区科学技术委员会医学卫生项目[21-E-62]。
