HPLC法同时测定风湿关节炎片中4种成分的含量
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篇名: HPLC法同时测定风湿关节炎片中4种成分的含量
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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pH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10 μl。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 0 μg/ml(r=0.999 6)、10.034~200.680 0 μg/ml(r=0.999 7)、8.693~121.700 0 μg/ml(r=0.999 9)、9.696~193.920 0 μg/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。
ABSTRACT: 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 heptanesulfonate 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 nm for ephedrine hydrochloride and pseudoephedrine hydrochloride, 260 nm for brucine and strychnine, column temperature was 30℃, and injection volume was 10 μl. RESULTS: The linear range was 0.916-18.320 0 μg/ml for pseudoephedrine 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 arthritis tablet.
期刊: 2016年第27卷第33期
作者: 逯雯洁,刘亚蓉,韩晓萍,刘学良
AUTHORS: LU Wenjie,LIU Yarong,HAN Xiaoping,LIU Xueliang
关键字: 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
KEYWORDS: HPLC; Rheumatoid arthritis tablet; Ephedrine hydrochloride; Pseudoephedrine hydrochloride; Brucine; Strychnine; Content determination
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