复方芦丁片溶出度测定方法的研究
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摘要
目的:建立测定复方芦丁片溶出度的方法。方法:采用HALO5-C18色谱柱(250 mm×4.6 mm,5μm),甲醇-0.4%磷酸溶液(60∶40)(用三乙胺调节pH值至3.0)为流动相;流速1.0ml/min;检测波长254nm。按《中华人民共和国药典》2015年版四部溶出度测定第一法(篮法),采用ERWEKA DT800智能药物溶出仪,通过对溶出介质、转速和取样时间的选择,确定复方芦丁片溶出度测定方法。结果:在本研究建立的色谱条件下,芦丁与维生素C分离度良好。芦丁的线性范围为5.0~40μg/ml(r=0.999 9);维生素C的线性范围为12.5~100μg/ml(r=1.000 0)。样品的溶出度均一性好,以pH 8.0磷酸盐缓冲液作为芦丁溶出介质,0.1mol/L盐酸溶液作为维生素C溶出介质,芦丁取样时间为45min,维生素C取样时间为30min,转速为100r/min。溶出限度均为不低于标示量的80%。结论:本研究建立的方法可用于复方芦丁片溶出度测定,能有效控制药品质量,为提高复方芦丁片质量标准提供依据。
Objective:To develop a method for the determination of the dissolution of compound Rutin tablets.Methods:The chromatographic analysis was carried out on a HALO5-C18column(250mm×4.6mm,5μm)with methanol-0.4% phosphate solution(60∶40)(pH adjusted to 3.0with trimethylamine)as mobile phase.The flow rate was 1.0ml/min and the detection wavelength was 254 nm.According to the first dissolution method(basket method)described in the Pharmacopoeia of the People's Republic of China(2015Edition,Volume 4),the dissolution determination conditions were established using ERWEKA DT800 intelligent drug dissolution instrument,and dissolution medium,rotational speed and sampling time were selected.Results:Rutin and vitamin C could be separated completely under the established chromatographic conditions.The linear ranges of Rutin and vitamin C were 5.0-40μg/ml(r=0.999 9)and 12.5-100μg/ml(r=1.000 0),respectively.The dissolution rates of the samples were consistent.The pH 8.0phosphate buffer solution and 0.1mol/L HCl solution were selected as release media for Rutin and vitamin C,respectively,rotational speed was 100r/min,the sampling time points were 45 and 30min for Rutin and vitamin C,respectively.The dissolution limit was not less than 80% of the labeled amount.Conclusion:This established method could be used for the dissolution determination and the quality control,and provide reference for the improvement of quality standards of compound Rutin tablets.
Objective:To develop a method for the determination of the dissolution of compound Rutin tablets.Methods:The chromatographic analysis was carried out on a HALO5-C18column(250mm×4.6mm,5μm)with methanol-0.4% phosphate solution(60∶40)(pH adjusted to 3.0with trimethylamine)as mobile phase.The flow rate was 1.0ml/min and the detection wavelength was 254 nm.According to the first dissolution method(basket method)described in the Pharmacopoeia of the People's Republic of China(2015Edition,Volume 4),the dissolution determination conditions were established using ERWEKA DT800 intelligent drug dissolution instrument,and dissolution medium,rotational speed and sampling time were selected.Results:Rutin and vitamin C could be separated completely under the established chromatographic conditions.The linear ranges of Rutin and vitamin C were 5.0-40μg/ml(r=0.999 9)and 12.5-100μg/ml(r=1.000 0),respectively.The dissolution rates of the samples were consistent.The pH 8.0phosphate buffer solution and 0.1mol/L HCl solution were selected as release media for Rutin and vitamin C,respectively,rotational speed was 100r/min,the sampling time points were 45 and 30min for Rutin and vitamin C,respectively.The dissolution limit was not less than 80% of the labeled amount.Conclusion:This established method could be used for the dissolution determination and the quality control,and provide reference for the improvement of quality standards of compound Rutin tablets.
引文
[1]中华人民共和国卫生部药典委员会.中华人民共和国卫生部药品标准化学药品及制剂:第一册[M].北京:人民卫生出版社,1989:88.Pharmacopoeia Committee of the Ministry of Public Health of the People’s Republic of China.Drug standards of the Ministry of Public Health of the People’s Republic of China.The chemical medicine and preparation:Volume 1[M].Beijing:People’s Health Press,1989:88.In Chinese.
[2]王艳,相秉仁.小波变换分光光度法同时测定复方芦丁片中芦丁和维生素C[J].理化检验:化学分册,2007,43(10):863-865.WANG Yan,XIANG BingRen.Simultaneous spectrophotometric determination of Rutin and vitamin C in Rutin compound tablets with wavelet transform[J].Physic Testing Chem Anal Part B:Chem Anal,2007,43(10):863-865.In Chinese with English abstract.
[3]孙银华.双波长高效液相色谱法测定复方芦丁片中维生素C和芦丁的含量[J].安徽医药,2012,16(1):30-32.SUN YinHua.Determination of vitamin C and Rutin in compound Rutin tablets by HPLC with dual-wavelength[J].Anhui Med Pharm J,2012,16(1):30-32.In Chinese with English abstract.
[4]马君义,张串霞,赵保堂.RP-HPLC法测定不同厂家芦丁片和复方芦丁片中芦丁的含量[J].西北师范大学学报(自然科学版),2010,46(5):74-77.MA JunYi,ZHANG ChuanXia,ZHAO BaoTang.Determination of Rutin in Rutin tablets and compound Rutin tablets from different manufacturers by RP-HPLC[J].J Northwest Normal Univ(Nat Sci),2010,46(5):74-77.In Chinese with English abstract.
[5]宋玉英,付鑫,贾首时.HPLC法测定芦丁片的含量和有关物质[J].中国药师,2010,13(8):1216-1217.SONG YuYing,FU Xin,JIA ShouShi.Determination of contents and related substances in Rutin tablets by HPLC method[J].China Pharmacist,2010,13(8):1216-1217.In Chinese.
[6]王克森,徐传新,程明,等.复方芦丁片中芦丁的溶出度考察[J].中国医院药学杂志,1992,12(10):450-451.In Chinese.WANG KeSen,XU ChuanXin,CHENG Ming,et al.Study on the dissolution rate of Rutin from compound Rutin tablets[J].Chin J Hosp Pharm,1992,12(10):450-451.In Chinese with English abstract.
[7]代龙.HPLC同时测定珍菊降压片中氢氯噻嗪与芦丁的含量[J].安徽医药,2009,13(5):510-511.DAI Long.Determination of hydrochlorothiazide and Rutin in Zhenjujiangya tablet by HPLC[J].Anhui Med Pharm J,2009,13(5):510-511.In Chinese with English abstract.
[8]田磊.HPLC法同时测定复方银翘氨敏胶囊中维生素C及对乙酰氨基酚的含量[J].安徽医药,2010,14(9):1026-1027.TIAN Lei.Simultaneous determination of vitamin C and paracetamol in Compound Yinqiao Anmin capsules by HPLC[J].Anhui Med Pharm J,2010,14(9):1026-1027.In Chinese with English abstract.
[9]刘波,张浩科,宫海燕.反相高效液相色谱法测定新疆枸杞叶茶中芦丁和槲皮素的含量[J].中国实验方剂学杂志,2011,17(14):92-94.LIU Bo,ZHANG HaoKe,GONG HaiYan.Determination of Rutin and quercetin in tea of Lycium barbarum leaves by RP-HPLC[J].Chin J Exp Tradit Med Formul,2011,17(14):92-94.In Chinese with English abstract.
[2]王艳,相秉仁.小波变换分光光度法同时测定复方芦丁片中芦丁和维生素C[J].理化检验:化学分册,2007,43(10):863-865.WANG Yan,XIANG BingRen.Simultaneous spectrophotometric determination of Rutin and vitamin C in Rutin compound tablets with wavelet transform[J].Physic Testing Chem Anal Part B:Chem Anal,2007,43(10):863-865.In Chinese with English abstract.
[3]孙银华.双波长高效液相色谱法测定复方芦丁片中维生素C和芦丁的含量[J].安徽医药,2012,16(1):30-32.SUN YinHua.Determination of vitamin C and Rutin in compound Rutin tablets by HPLC with dual-wavelength[J].Anhui Med Pharm J,2012,16(1):30-32.In Chinese with English abstract.
[4]马君义,张串霞,赵保堂.RP-HPLC法测定不同厂家芦丁片和复方芦丁片中芦丁的含量[J].西北师范大学学报(自然科学版),2010,46(5):74-77.MA JunYi,ZHANG ChuanXia,ZHAO BaoTang.Determination of Rutin in Rutin tablets and compound Rutin tablets from different manufacturers by RP-HPLC[J].J Northwest Normal Univ(Nat Sci),2010,46(5):74-77.In Chinese with English abstract.
[5]宋玉英,付鑫,贾首时.HPLC法测定芦丁片的含量和有关物质[J].中国药师,2010,13(8):1216-1217.SONG YuYing,FU Xin,JIA ShouShi.Determination of contents and related substances in Rutin tablets by HPLC method[J].China Pharmacist,2010,13(8):1216-1217.In Chinese.
[6]王克森,徐传新,程明,等.复方芦丁片中芦丁的溶出度考察[J].中国医院药学杂志,1992,12(10):450-451.In Chinese.WANG KeSen,XU ChuanXin,CHENG Ming,et al.Study on the dissolution rate of Rutin from compound Rutin tablets[J].Chin J Hosp Pharm,1992,12(10):450-451.In Chinese with English abstract.
[7]代龙.HPLC同时测定珍菊降压片中氢氯噻嗪与芦丁的含量[J].安徽医药,2009,13(5):510-511.DAI Long.Determination of hydrochlorothiazide and Rutin in Zhenjujiangya tablet by HPLC[J].Anhui Med Pharm J,2009,13(5):510-511.In Chinese with English abstract.
[8]田磊.HPLC法同时测定复方银翘氨敏胶囊中维生素C及对乙酰氨基酚的含量[J].安徽医药,2010,14(9):1026-1027.TIAN Lei.Simultaneous determination of vitamin C and paracetamol in Compound Yinqiao Anmin capsules by HPLC[J].Anhui Med Pharm J,2010,14(9):1026-1027.In Chinese with English abstract.
[9]刘波,张浩科,宫海燕.反相高效液相色谱法测定新疆枸杞叶茶中芦丁和槲皮素的含量[J].中国实验方剂学杂志,2011,17(14):92-94.LIU Bo,ZHANG HaoKe,GONG HaiYan.Determination of Rutin and quercetin in tea of Lycium barbarum leaves by RP-HPLC[J].Chin J Exp Tradit Med Formul,2011,17(14):92-94.In Chinese with English abstract.