HPLC波长切换法同时测定清骨解毒生血丸中4种指标成分  

Simultaneous Determination of 4 Active Components in Qinggu Jiedu Shengxue Pills by HPLC Wavelength Switching Method

作　　者：刘海燕 魏佩尧 童蒙蒙 LIU Hai-yan;WEI Pei-yao;TONG Meng-meng(Zhoukou Institute for Food and Drug Control,Zhoukou 466000,China;Xiaoqiao Community Health Service Center,Chuanhui District,Zhoukou City,Zhoukou 466000,China)

机构地区：[1]河南省周口市食品药品检验所,河南周口466000 [2]河南省周口市川汇区小桥社区卫生服务中心,河南周口466000

出　　处：《食品与药品》2019年第6期486-490,共5页Food and Drug

摘　　要：目的建立HPLC波长切换法同时测定清骨解毒生血丸中梓醇、芍药苷、毛蕊花糖苷和丹皮酚含量的方法。方法采用Waters Symmetry-C18(250 mm×4.6 mm,5μm)色谱柱;以乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱;流速:1.0 ml/min;梓醇的检测波长为210 nm(0~15 min),芍药苷的检测波长为230 nm(15~28 min),毛蕊花糖苷的检测波长为334 nm(28~40 min),丹皮酚的检测波长为274 nm(40~52 min);进样量:10μl;柱温:30℃。结果4种被测成分分离度良好,梓醇、芍药苷、毛蕊花糖苷和丹皮酚的进样量分别在0.04502~0.6753μg(r=0.9996),0.04028~0.6042μg(r=0.9998),0.01512~0.2268μg(r=0.9999)和0.08561~1.2842μg(r=0.9999)的范围内呈良好线性关系;精密度、稳定性、重复性试验的RSD均小于2%;平均加样回收率(n=6)分别为97.89%(RSD=0.92%),98.51%(RSD=0.86%),97.87%(RSD=1.13%)和98.88%(RSD=0.63%)。结论该方法可靠、准确、重复性好,为全面评价清骨解毒生血丸的质量提供技术参考。Objective To establish an HPLC wavelength switching method for the simultaneous determination of catalpol,paeoniflorin,mulberry glycoside and paeonol in Qinggu Jiedu Shengxue Pills.Methods The chromatographic separation was carried out on a Waters Symmetry-C18 column(250 mm×4.6 mm,5μm).Gradient elution mode was used,with acetonitrile(A)-0.1%phosphoric acid solution(B)at the flow rate of 1.0 ml/min as mobile phase.The UV detection wavelengths of catalpol,paeoniflorin,mulberry glycoside and paeonol were set at 210 nm(0-15 min),230 nm(15-28 min),334 nm(28-40 min)and 274 nm(40-52 min),respectively.The injection volume was 10μl and the column temperature was 30℃.Results Excellent chromatographic separation was achieved and the linear ranges for catalpol,paeoniflorin,mulberry glycoside and paeonol were 0.04502-0.6753μg(r=0.9996),0.04028-0.6042μg(r=0.9998),0.01512-0.2268μg(r=0.9999)and 0.08561-1.2842μg(r=0.9999),respectively.The relative standard deviations(RSDs)of precision,stability and repeatability were less than 2%.The average recoveries(n=6)were 97.89%(RSD=0.92%),98.51%(RSD=0.86%),97.87%(RSD=1.13%)and 98.88%(RSD=0.63%),respectively.Conclusion The method is reliable,accurate and reproducible,and it can provide technical reference for the comprehensive evaluation of the quality of Qinggu Jiedu Shengxue Pills.

关 键 词：清骨解毒生血丸 梓醇 芍药苷 毛蕊花糖苷 丹皮酚 HPLC 

分 类 号：R927.2[医药卫生—药学]