UPLC法同时测定黄连与代综方中4种生物碱的含量  

Simultaneous Determination of 4 Kinds of Alkaloids from Coptidis Rhizoma and Daizongfang by UPLC

作　　者：陈健龙[1,2] 张玉玲[1,2] 肖胜利[1] 崔翰明[1] 贡济宇[2] 

机构地区：[1]中国中医科学院广安门医院,北京100053 [2]长春中医药大学,长春130117

出　　处：《中国药房》2013年第23期2152-2154,共3页China Pharmacy

基　　金：国家科技重大新药创制专项资助课题(No.2011ZX09102-011-08)

摘　　要：目的:建立同时测定黄连与代综方中药根碱、黄连碱、巴马汀、小檗碱4种原小檗碱型生物碱含量的方法。方法:采用超高效液相色谱法。色谱柱为ACQUITY UPLC BEH C18(100mm×2.1mm,1.7μm),流动相为乙腈-水(含2mmol乙酸铵和0.05%甲酸,30∶70,V/V,pH3.20),流速为0.3ml/min,柱温为30℃,检测波长为345nm。结果:盐酸药根碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱的质量浓度分别在21.76～1088.05、20.88～1044.00、17.68～884.05、18.32～916.10ng/ml范围内与各自峰面积积分值呈良好的线性关系(r均为0.9999)。精密度、稳定性、重复性试验结果的RSD均<5%。平均加样回收率结果:(1)黄连:盐酸药根碱为101.56%,RSD=2.16%(n=6);盐酸黄连碱为100.21%,RSD=3.32%(n=6);盐酸巴马汀为97.60%,RSD=1.96%(n=6);盐酸小檗碱为98.81%,RSD=1.48%(n=6)。(2)代综方:盐酸药根碱为98.87%,RSD=2.41%(n=6);盐酸黄连碱为99.12%,RSD=2.68%(n=6);盐酸巴马汀为98.98%,RSD=2.23%(n=6);盐酸小檗碱为98.55%,RSD=2.82%(n=6)。最低检出限和最低定量限:盐酸药根碱分别为4.50、14.99ng/ml,盐酸黄连碱分别为5.10、17.00ng/ml,盐酸巴马汀分别为4.81、16.04ng/ml,盐酸小檗碱分别为4.64、15.47ng/ml。结论:该方法简便、灵敏、准确、高效,可用于黄连及其复方制剂的质量控制。OBJECTIVE： To establish the method for simultaneous determination of jatrorrhizine, coptisine, palmatine and ber-berine, ,t kinds of alkaloid in Coptidis Rhizoma and Daizongfang. METHODS： UPLC method was adopted. The determination was performed on ACQU1TY UPLC BEH C18（100mm×2.1mm,1.7μm） column with mobile phase consisted of acetonitrile-water （2 mmol ammonium acetate and 0.05% formic acid, 30：70, V/V, pH：3.20） at the flow rate of 0.3 ml/min. The column temperature was 30 ℃, and detection wavelength was 345 nm. RESULTS： The liner ranges ofjatrorrhizine, coptisine, palmatine and berberine hydrochloride were 21.76-1 088.05 ng/ml, 20.88-1 044.00 ng/ml, 17.68-884.05 ng/ml and 18.32-916.10 ng/ml （all r=0.999 9）, re-spectively. RSDs of precision, stability and reproducibility test were all lower than 5%. The average recoveries ofjatrorrhizine, cop- tisine, palmatine and berberine hydrochloride in Coptidis Rhizoma were 101.56% （RSD=2.16%） , 100.21% （RSD=3.32%） , 97.60% （RSD=1.96% ） and 98.81% （RSD= 1.48% ）, respectively （n=6）. The average recoveries of 4 alkaloids in Daizongfang were 98.87% （RSD=2.41%）, 99.12%（RSD：2.68%）,98.98%（RSD=2.23%）,98.55%（RSD=2.82%）, respectively（n=6）. The lowest detectable and quantitative concentration of 4 alkaloids were 4.50 and 14.99 ng/ml, 5.10 and 17.00 ng/ml,4.81 and 16.04 ng/ml, .1.64 and 15.47 ng/ml, respectively. CONCLUSIONS： The method is simple, accurate and reproducible. It can be used for the quality control of Coptidis Rhizoma and its component preparation.

关 键 词：超高效液相色谱法 黄连 代综方 药根碱 黄连碱 巴马汀 小檗碱 含量测定 

分 类 号：R283.64[医药卫生—中药学] R284.1[医药卫生—中医学]