基于多指标成分定量评价复方鱼腥草胶囊
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摘要
目的:基于多指标成分定量评价分析复方鱼腥草胶囊,为复方鱼腥草胶囊的质量控制提供参考。方法:首先制备复方鱼腥草胶囊供试品溶液及槲皮苷、表告依春、绿原酸、连翘苷、黄芩苷对照品溶液,色谱条件采用CAPCELL-PAK-MG-C_(18)色谱柱(5μm,规格:4. 6 mm×250 mm),柱温以35℃为宜,进样量为10μL,流速为1. 0 m L/min进行高效液相色谱(HPLC)检测,以流动相A(乙腈)和流动相B(水+0. 01%磷酸)为条件进行梯度洗脱,优化高效液相(HPLC)的方法学严谨性,进行线性回归、精密度、重复性、稳定性、专属性试验和加样回收率试验,多指标成分定量分析样品中槲皮苷、表告依春、绿原酸、连翘苷和黄芩苷的含量。结果:1)采用HPLC色谱法对复方鱼腥草胶囊中鱼腥草、板蓝根、金银花、连翘、黄芩等进行专属性试验,结果显示复方鱼腥草胶囊中鱼腥草、板蓝根、金银花、连翘、黄芩专属性良好。2)线性范围考察结果显示槲皮苷对照品、连翘苷对照品、绿原酸对照品在4～201μg/m L范围内、表告依春对照品、黄芩苷对照品在12～601μg/m L范围内的线性关系均良好。3)精密度试验结果显示槲皮苷、连翘苷、绿原酸、表告依春对照品、黄芩苷峰面积相对标准偏差(RSD)分别是0. 45%、0. 52%、0. 66%、0. 59%、0. 31%,结果表明此色谱条件下的HPLC仪器精密度良好。4)稳定性试验结果显示复方鱼腥草胶囊供试品溶液相对峰面积RSD是1. 33%,表明24 h内复方鱼腥草胶囊供试品溶液基本稳定。5)重复性试验结果显示复方鱼腥草胶囊供试品溶液相对峰面积RSD为0. 92%,表明该HPLC方法的重复性良好。6)结果显示槲皮苷、表告依春、绿原酸、连翘苷和黄芩苷的平均回收率分别为99. 10%、99. 26%、99. 07%、98. 05%、98. 82%、98. 32%,RSD为1. 81%、1. 49%、0. 94%、1. 58%、1. 01%,表明回收率较好。7)基于多指标成分定量测定结果显示不同厂家不同批次的复方鱼腥草胶囊中有效成分槲皮苷、表告依春、绿原酸、连翘苷和黄芩苷的含量存在较大差异。结论:基于多指标成分定量测定结果显示不同厂家不同批次的复方鱼腥草胶囊中有效成分槲皮苷、表告依春、绿原酸、连翘苷和黄芩苷的含量存在较大差异。
Objective: Based on the quantitative evaluation and analysis of compound Houttuynia cordata capsule based on multiindex components,it provides a reference for the quality control of compound Houttuynia cordata capsule. Methods: First,the compound Houttuynia capsule sample solution and quercetin were prepared,including Yichun,chlorogenic acid,forsythrin,baicalin reference solution,The chromatographic conditions were determined by high performance liquid chromatography( HPLC) with CAPCELL-PAK-MG-C18 column( 5 μm,specification: 4. 6 mm × 250 mm),column temperature 35 ℃,injection volume 10 μL,flow rate 1. 0 m L/min). Gradient eluting was carried out under the conditions of mobile phase A( acetonitrile) and mobile phase B( water 0. 01% phosphate). Optimize the methodological rigour of high performance liquid phase( HPLC),carry out linear regression,precision,reproducibility,stability,specificity test and sample recovery test,quantitative analysis of quercetin in samples with multiple index components,Quercetin,chlorogenic acid,The contents of phillyrin and baicalin. Results: 1) the specific tests of Houttuynia cordata,Radix Isatidis,Flos Lonicerae,Forsythia suspensa and Scutellaria baicalensis were carried out by HPLC chromatography. the results showed that Houttuynia cordata,Radix Isatidis,Flos Lonicerae and Forsythia suspensa were found in the compound Houttuynia cordata capsule. Scutellaria baicalensis Georgi has a good specificity. 2) the linear range of quercetin,phillyrin and chlorogenic acid were within the range of 4≤201 μg/m L,and the linear range of baicalin and baicalin were 12 μg/m L and 601 μg/m L,respectively. the linear range of quercetin,phillyrin and chlorogenic acid was 4≤201 μg/m L. 3) the results of precision test showed that the relative standard deviation( RSD) of quercetin,phillyrin,chlorogenic acid and baicalin peak area were 0. 45%,0. 52%,0. 66%,0. 59%,0. 31%,0. 51%,0. 52%,0. 56%,0. 59%,0. 31%,0. 52%,0. 62%,0. 59% and0. 31%,respectively. The results show that the precision of HPLC instrument under this chromatographic condition is good. 4)The results of stability test showed that the relative peak area RSD of compound Houttuynia capsule solution was 1. 33%,which indicated that the solution of compound Houttuynia capsule was basically stable within 24 hours. 5) The results of reproducibility test showed that the relative peak area RSD of compound Houttuynia capsule solution was 0. 92%,which indicated that the HPLC method had good reproducibility. 6) The results showed that the average recovery of quercetin,eichun,chlorogenic acid,phillyrin and baicalin were 99. 10%,99. 26%,99. 07%,98. 05%,98. 82%,98. 32%,1. 81% and 1. 49%,respectively. 0. 94%,1. 58%,1. 01%,indicating that the recovery is good. 7) The results of quantitative determination based on multi-index components showed that the contents of quercetin,chlorogenic acid,phillyrin and baicalin in different batches of compound Houttuynia cordata Thunb capsules from different manufacturers were quite different. Conclusion: The results of quantitative determination based on multi-index components showed that the contents of quercetin,chlorogenic acid,phillyrin and baicalin in different batches of compound Houttuynia cordata Thunb capsules from different manufacturers were quite different.
Objective: Based on the quantitative evaluation and analysis of compound Houttuynia cordata capsule based on multiindex components,it provides a reference for the quality control of compound Houttuynia cordata capsule. Methods: First,the compound Houttuynia capsule sample solution and quercetin were prepared,including Yichun,chlorogenic acid,forsythrin,baicalin reference solution,The chromatographic conditions were determined by high performance liquid chromatography( HPLC) with CAPCELL-PAK-MG-C18 column( 5 μm,specification: 4. 6 mm × 250 mm),column temperature 35 ℃,injection volume 10 μL,flow rate 1. 0 m L/min). Gradient eluting was carried out under the conditions of mobile phase A( acetonitrile) and mobile phase B( water 0. 01% phosphate). Optimize the methodological rigour of high performance liquid phase( HPLC),carry out linear regression,precision,reproducibility,stability,specificity test and sample recovery test,quantitative analysis of quercetin in samples with multiple index components,Quercetin,chlorogenic acid,The contents of phillyrin and baicalin. Results: 1) the specific tests of Houttuynia cordata,Radix Isatidis,Flos Lonicerae,Forsythia suspensa and Scutellaria baicalensis were carried out by HPLC chromatography. the results showed that Houttuynia cordata,Radix Isatidis,Flos Lonicerae and Forsythia suspensa were found in the compound Houttuynia cordata capsule. Scutellaria baicalensis Georgi has a good specificity. 2) the linear range of quercetin,phillyrin and chlorogenic acid were within the range of 4≤201 μg/m L,and the linear range of baicalin and baicalin were 12 μg/m L and 601 μg/m L,respectively. the linear range of quercetin,phillyrin and chlorogenic acid was 4≤201 μg/m L. 3) the results of precision test showed that the relative standard deviation( RSD) of quercetin,phillyrin,chlorogenic acid and baicalin peak area were 0. 45%,0. 52%,0. 66%,0. 59%,0. 31%,0. 51%,0. 52%,0. 56%,0. 59%,0. 31%,0. 52%,0. 62%,0. 59% and0. 31%,respectively. The results show that the precision of HPLC instrument under this chromatographic condition is good. 4)The results of stability test showed that the relative peak area RSD of compound Houttuynia capsule solution was 1. 33%,which indicated that the solution of compound Houttuynia capsule was basically stable within 24 hours. 5) The results of reproducibility test showed that the relative peak area RSD of compound Houttuynia capsule solution was 0. 92%,which indicated that the HPLC method had good reproducibility. 6) The results showed that the average recovery of quercetin,eichun,chlorogenic acid,phillyrin and baicalin were 99. 10%,99. 26%,99. 07%,98. 05%,98. 82%,98. 32%,1. 81% and 1. 49%,respectively. 0. 94%,1. 58%,1. 01%,indicating that the recovery is good. 7) The results of quantitative determination based on multi-index components showed that the contents of quercetin,chlorogenic acid,phillyrin and baicalin in different batches of compound Houttuynia cordata Thunb capsules from different manufacturers were quite different. Conclusion: The results of quantitative determination based on multi-index components showed that the contents of quercetin,chlorogenic acid,phillyrin and baicalin in different batches of compound Houttuynia cordata Thunb capsules from different manufacturers were quite different.
引文
[1]李金玉.复方鱼腥草片中绿原酸、黄芩苷的测定及指纹图谱的建立[J].中国实验方剂学杂志,2014,56(12):65-69.
[2]游思湘,符晨星,瞿俊勇,等.复方鱼腥草制剂的体外抑菌及耐药抑制作用研究[J].中国兽医杂志,2014,33(11):63-66.
[3]张华静.复方鱼腥草颗粒治疗小儿急性扁桃体炎风热证的临床研究[J].医学理论与实践,2013,26(2):194-195.
[4]史耀勋.复方鱼腥草滴丸治疗慢性肾炎合并急性咽炎、扁桃体炎[J].中国民间疗法,2014,22(8):48-49.
[5]李莹,秦献辉,李旭东,等.复方鱼腥草胶囊抗炎作用及机制实验研究[J].沈阳药科大学学报,2004,21(5):371-373,388.
[6]罗璇,李小芩,杨岳隆,等.复方鱼腥草软胶囊的鉴别和含量测定方法研究[J].中国中药杂志,2004,29(7):702-704.
[7]关潇滢,陈雪莲,王淑红,等.HPLC同时测定复方鱼腥草片中4个有效成分的含量[J].中国现代应用药学,2017,31(9):1300-1303.
[8]余星云,欧荔枝.复方鱼腥草滴丸中黄芩苷的HPLC含量测定[J].今日药学,2011,21(7):437-439.
[9]黄舒丽.复方鱼腥草软胶囊中(R,S)-告依春含量测定方法的研究[J].中国医药导报,2011,8(35):70-72.
[10]虞利东,吴健,徐斌,等.复方鱼腥草合剂中连翘苷的含量测定?[J].医药导报,2016,35(z1):93-94.
[11]曹金枝,苏志刚.HPLC法测定复方鱼腥草片中绿原酸的含量[J].首都医药,2014,18(20):93-94.
[12]李莹,秦献辉,李旭东,等.复方鱼腥草胶囊的抗炎及免疫功能调节作用[J].沈阳药科大学学报,2004,21(4):297-300.
[13]匡钊.高效液相色谱法测定复方鱼腥草颗粒中黄芩苷和黄芩素含量[J].安徽中医药大学学报,2016,35(6):91-94.
[14]李金玉.复方鱼腥草片中绿原酸、黄芩苷的测定及指纹图谱的建立[J].中国实验方剂学杂志,2014,54(12):65-69.
[2]游思湘,符晨星,瞿俊勇,等.复方鱼腥草制剂的体外抑菌及耐药抑制作用研究[J].中国兽医杂志,2014,33(11):63-66.
[3]张华静.复方鱼腥草颗粒治疗小儿急性扁桃体炎风热证的临床研究[J].医学理论与实践,2013,26(2):194-195.
[4]史耀勋.复方鱼腥草滴丸治疗慢性肾炎合并急性咽炎、扁桃体炎[J].中国民间疗法,2014,22(8):48-49.
[5]李莹,秦献辉,李旭东,等.复方鱼腥草胶囊抗炎作用及机制实验研究[J].沈阳药科大学学报,2004,21(5):371-373,388.
[6]罗璇,李小芩,杨岳隆,等.复方鱼腥草软胶囊的鉴别和含量测定方法研究[J].中国中药杂志,2004,29(7):702-704.
[7]关潇滢,陈雪莲,王淑红,等.HPLC同时测定复方鱼腥草片中4个有效成分的含量[J].中国现代应用药学,2017,31(9):1300-1303.
[8]余星云,欧荔枝.复方鱼腥草滴丸中黄芩苷的HPLC含量测定[J].今日药学,2011,21(7):437-439.
[9]黄舒丽.复方鱼腥草软胶囊中(R,S)-告依春含量测定方法的研究[J].中国医药导报,2011,8(35):70-72.
[10]虞利东,吴健,徐斌,等.复方鱼腥草合剂中连翘苷的含量测定?[J].医药导报,2016,35(z1):93-94.
[11]曹金枝,苏志刚.HPLC法测定复方鱼腥草片中绿原酸的含量[J].首都医药,2014,18(20):93-94.
[12]李莹,秦献辉,李旭东,等.复方鱼腥草胶囊的抗炎及免疫功能调节作用[J].沈阳药科大学学报,2004,21(4):297-300.
[13]匡钊.高效液相色谱法测定复方鱼腥草颗粒中黄芩苷和黄芩素含量[J].安徽中医药大学学报,2016,35(6):91-94.
[14]李金玉.复方鱼腥草片中绿原酸、黄芩苷的测定及指纹图谱的建立[J].中国实验方剂学杂志,2014,54(12):65-69.