高效液相色谱法测定盐酸吗啉胍片含量及其不确定度评定  

Content Determination of Moroxydine Hydrochloride in Moroxydine Hydrochloride Tablets by HPLC and Evaluation of Its Uncertainty

作　　者：朱清丽 李鹏 郭梦倩 涂蓉荣 ZHU Qingli;LI Peng;GUO Mengqian;TU Rongrong(Ankang Institute for Food and Drug Control,Ankang,Shaanxi,China 725000;Ankang Central Hospital,Ankang,Shaanxi,China 725000)

机构地区：[1]陕西省安康市食品药品检验检测中心,陕西安康725000 [2]陕西省安康市中心医院,陕西安康725000

出　　处：《中国药业》2021年第18期60-64,共5页China Pharmaceuticals

摘　　要：目的建立测定盐酸吗啉胍片含量的高效液相色谱法,并评定其不确定度。方法色谱柱为Phenomenex C_(18)柱(250mm×4.6mm,5μm),流动相为0.2mol/L磷酸二氢钾溶液-甲醇(95∶5,V/V),流速为1.0mL/min,检测波长为237nm,柱温为30℃,进样量为20μL。并通过建立此方法测定数学模型,分析测量过程,确定不确定度来源和合成不确定度(UC)。结果盐酸吗啉胍质量浓度在2~20μg/mL范围内与峰面积线性关系良好(r=0.9999,n=6),平均回收率为100.72%,RSD为0.63%(n=9);样品含量测定结果低于现行紫外-可见分光光度法的测定结果,其Uc为0.43%,扩展不确定度(U)为0.86%(k=2)。结论通过不确定度评定,相较样品现行标准检测方法,所建立的高效液相色谱法专属性更强、重复性更好、准确度更高,可用于盐酸吗啉胍片的质量控制。Objective To establish a high-performance liquid chromatography(HPLC)method for the content determination of moroxyguanidine hydrochloride in Moroxyguanidine Hydrochloride Tablets and evaluate its uncertainty.Methods The chromatographic column was Phenomenex C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was 0.2 mol/L potassium dihydrogen phosphate solution-methanol(95∶5,V/V),the flow rate was 1.0 m L/min,the detection wavelength was 237 nm,the column temperature was 30℃,and the injection volume was 20μL.Through the establishment of this method,the mathematical model was determined,the measurement process was analyzed,and the source of uncertainty and scombined uncertainty(UC)were determined.Results The linear range of moroxydine hydrochloride was 2-20μg/m L(r=0.9999,n=6),the average recovery of moroxydine hydrochloride was 100.72%with RSD of 0.63%(n=9).The content of moroxydine hydrochloride in the sample determined by this method was lower than that determined by the current UV-VIS spectrophotometry,the UC was 0.43%and the expanded uncertainty(U)was 0.86%(k=2).Conclusion Through the evaluation of uncertainty,the established HPLC method has stronger specificity,better repeatability and higher accuracy than the current standard determination method,it can be used for the quality control of Moroxydine Hydrochloride Tablets.

关 键 词：高效液相色谱法 盐酸吗啉胍片 含量测定 不确定度 

分 类 号：R927.2[医药卫生—药学]