复方芦丁片溶出度测定方法的建立及应用  

Establishment and Application of a Dissolution Determination Method for Compound Rutin Tablets

作　　者：屈晓萍 屠相土 李俊 QU Xiaoping;TU Xiangtu;LI Jun(Zhejiang Taizhou Institute for Drug Control,Taizhou,Zhejiang,China 318000)

机构地区：[1]浙江省台州市药品检验研究院,浙江台州318000

出　　处：《中国药业》2023年第18期81-84,共4页China Pharmaceuticals

基　　金：浙江省台州市社会发展类科技计划项目[22ywb90]。

摘　　要：目的建立复方芦丁片溶出度的测定方法,并以此评价国内市售产品的质量。方法采用高效液相色谱法,色谱柱为PolyPak C18柱(250 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(pH 3.0)-甲醇(55∶45,V/V),流速为1.0 mL/min,检测波长为259 nm,柱温为30℃,进样量为20μL。以累积溶出度为考察指标,采用单因素试验优选转速、十二烷基二甲基氧化胺(LDAO)溶液体积分数,并考察取样时间和管路吸附对其的影响。结果芦丁质量浓度在1.103~33.090μg/mL(r=0.9999,n=8)范围内与峰面积线性关系良好;定量限为0.180μg/mL,检测限为0.055μg/mL;精密度、稳定性、重复性试验结果的RSD均小于1.0%;平均加样回收率为100.70%,RSD为1.76%(n=9);样品以0.5%LDAO溶液(900 mL)为溶出介质、转速为75 r/min,在45 min时取样可得较好累积溶出度。5家企业27批样品的溶出度,1家有2批在70%~75%之间,1家各批均低于70%。结论所建立的方法专属性强,精密度、稳定性、重复性和准确度好,能反映国内不同企业所产复方芦丁片的质量差异。Objective To establish a method for determining the dissolution of Compound Rutin Tablets,and on this basis,to evaluate the quality of commercial products in China.Methods High-performance liquid chromatography(HPLC)method was adopted,the chromatographic column was PolyPak C18 column(250 mm×4.6 mm,5μm),the mobile phase was phosphate buffer(pH 3.0)-methanol(55∶45,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 259 nm,the column temperature was 30℃,and the injection volume was 20μL.With the cumulative dissolution as the evaluation index,the rotational speed and volume fraction of lauryl dimethylamine oxide(LDAO)solution were optimized by the single factor test,and the effects of sampling time and pipeline adsorption on the cumulative dissolution were investigated.Results The linear range of rutin was 1.103-33.090μg/mL(r=0.9999,n=8).The limit of quantification was 0.180μg/mL,and the limit of detection was 0.055μg/mL.The RSDs of precision,stability and repeatability tests were all lower than 1.0%.The average recovery rate of rutin was 100.70%with an RSD of 1.76%(n=9).The optimal dissolution determination method was as follows:0.5%LDAO solution(900 mL)was as the dissolution medium,the rotational speed was 75 r/min,and the sampling time was 45 min.Among the 27 batches of samples(five enterprises),the dissolution of two batches(one enterprise)was in the range of 70%to 75%,while that of all batches(another enterprise)was below 70%.Conclusion The established method is specific,precise,stable,repeatable and accurate,which can display the quality differences of Compound Rutin Tablets produced by different enterprises in China.

关 键 词：复方芦丁片 高效液相色谱法 溶出度 质量评价 

分 类 号：R927.1[医药卫生—药学]