HPLC法同时测定风湿关节炎片中4种成分的含量  

Simultaneous Setermination of Four Components of Rheumatoid Arthritis Tablet by HPLC

作　　者：逯雯洁 刘亚蓉 韩晓萍 刘学良 

机构地区：[1]青海省药品检验检测院,西宁810016

出　　处：《中国药房》2016年第33期4692-4695,共4页China Pharmacy

基　　金：国家药品计划抽验项目(No.2014)

摘　　要：目的：建立同时测定风湿关节炎片中盐酸麻黄碱、盐酸伪麻黄碱、马钱子碱、士的宁含量的方法。方法：采用高效液相色谱法。色谱柱为XTerra-C18,流动相为乙腈-0.01 mol/L庚烷磺酸钠与0.01 mol/L磷酸二氢钾的等量混合溶液（用磷酸调p H至2.8）（梯度洗脱）,流速为1.0 ml/min,检测波长为206 nm（盐酸麻黄碱和盐酸伪麻黄碱）、260 nm（马钱子碱和士的宁）,柱温为30℃,进样量为10μl。结果：盐酸伪麻黄碱、盐酸麻黄碱、马钱子碱和士的宁检测质量浓度线性范围分别为0.916-18.320 0μg/ml（r=0.999 6）、10.034-200.680 0μg/ml（r=0.999 7）、8.693-121.700 0μg/ml（r=0.999 9）、9.696-193.920 0μg/ml（r=0.999 9）;定量限分别为0.03、0.07、0.04、0.03 ng,检测限分别为0.01、0.02、0.01、0.01 ng;精密度、稳定性、重复性试验的RSD〈2.0%;加样回收率分别为97.30%-99.79%（RSD=0.96%,n=6）、95.81%-99.36%（RSD=0.38%,n=6）、95.34%-99.93%（RSD=2.00%,n=6）、95.59%-99.80%（RSD=1.76%,n=6）。结论：该方法操作简便、结果准确,可用于同时测定风湿关节炎片中盐酸麻黄碱、盐酸伪麻黄碱、马钱子碱、士的宁的含量。OBJECTIVE： To establish a method for simultaneous determination of ephedrine hydrochloride, pseudoephedrine hydrochloride, brucine, strychnine in Rheumatoid arthritis tablet. METHODS： HPLC was performed on column of XTerra-C18 with mobile phase of acetonitrile-mixed solution （pH was adjusted to 2.8 with phosphate acid） composing of 0.01 mol/L sodium heptane- sulfonate solution and equal quantity of 0.01 mol/L potassium dihydrogen phosphate solution at a flow rate of 1.0 ml/min, detection wavelength was 206 mn for ephedrine hydrochloride and pseudoephedrine hydrochloride, 260 mn for brucine and strychnine, col- umn temperature was 30℃, and injection volume was 10 μl. RESULTS： The linear range was 0.916-18.320 0μg/ml for pseudo- ephedrine hydrochloride （r=0.999 6）, 10.034-200.680 0 μg/ml for ephedrine hydrochloride（r=0.999 7）, 8.693-121.700 0 μg/ml for brucine（r=0.999 9） and 9.696-193.920 0 μg/ml for strychnine（r=0.999 9）; limits of quantification were 0.03, 0.07, 0.04, 0.03 ng, limits of detection were 0.01, 0.02, 0.01, 0.01 ng; RSDs of precision, stability and reproducibility tests were lower than 2.0% ; recoveries were 97.30%-99.79% （RSD=0.96%, n=6）, 95.81%-99.36% （RSD=0.38%, n=6）, 95.34%-99.93% （RSD= 2.00% ,n=6） and 95.59%-99.80%（RSD=1.76% ,n=6）. CONCLUSIONS： The method is simple, accurate, and can be used for the simultaneous determination of ephedrine hydrochloride, pseudoephedrine hydrochloride, brucine, strychnine in Rheumatoid ar- thritis tablet.

关 键 词：高效液相色谱法 风湿关节炎片 盐酸麻黄碱、盐酸伪麻黄碱、马钱子碱、士的宁 含量测定 

分 类 号：R927.2[医药卫生—药学]