基于HPLC-QQQ/MS的龙生蛭胶囊中19种代表性成分含量一致性分析
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摘要
龙生蛭胶囊是由12味中药组成临床上广泛应用于脑梗死恢复期治疗的复方制剂,为考察其制剂批次间含量的一致性,该文选择龙生蛭胶囊19种代表性成分,建立高效液相色谱-三重串联四极杆质谱分析法,实现了9 min内的快速定量分析。方法学考察结果表明,该分析方法简单、快速、灵敏度高、重复性好,可用于对龙生蛭胶囊制剂成分的含量测定。制剂批次间一致性分析结果表明,制剂中化学成分以芍药苷和毛蕊异黄酮葡糖苷含量最高,不同批次制剂之间19个化合物总含量一致性好,RSD为5. 2%,其中主成分黄芪甲苷、毛蕊异黄酮葡糖苷等化合物的RSD均小于15%,也具较好一致性。研究结果为龙生蛭胶囊制剂的质量控制和一致性评价提供科学方法及依据。
Longshengzhi capsule consisting of 12 herbs is widely used in clinically treating cerebral ischemia during recovery period.In this study,in order to investigate the consistency of different batches of Longshengzhi capsules,a high performance liquid chromatography coupled to triple quadrupole mass spectrometry method(HPLC-QQQ/MS) was developed for the determination of 19 representative components in Longshengzhi Capsules within 9 min. Methodology validation indicated this method was simple,rapid,accurate,highly sensitive and reproducible,and it could be used for the content determination of components in Longshengzhi Capsules. The consistency analysis results showed that paeoniflorin and calycosin-7-glucoside in Longshengzhi Capsules had the highest content; RSD value of total content of 19 compounds was 5. 2% and the RSD value of main compounds such as astragaloside and calycosin-7-glucoside was all less than 15%,reflecting good consistency among different batches. This study has provided a scientific method and basis for the quality control and consistency evaluation of Longshengzhi Capsules.
Longshengzhi capsule consisting of 12 herbs is widely used in clinically treating cerebral ischemia during recovery period.In this study,in order to investigate the consistency of different batches of Longshengzhi capsules,a high performance liquid chromatography coupled to triple quadrupole mass spectrometry method(HPLC-QQQ/MS) was developed for the determination of 19 representative components in Longshengzhi Capsules within 9 min. Methodology validation indicated this method was simple,rapid,accurate,highly sensitive and reproducible,and it could be used for the content determination of components in Longshengzhi Capsules. The consistency analysis results showed that paeoniflorin and calycosin-7-glucoside in Longshengzhi Capsules had the highest content; RSD value of total content of 19 compounds was 5. 2% and the RSD value of main compounds such as astragaloside and calycosin-7-glucoside was all less than 15%,reflecting good consistency among different batches. This study has provided a scientific method and basis for the quality control and consistency evaluation of Longshengzhi Capsules.
引文
[1]冯哮龙.龙生蛭胶囊:中风恢复期疗效佳[J].医师在线,2018(2):31.
[2]杨桂林.联合应用龙生蛭胶囊和阿司匹林治疗短暂性脑缺血发作的效果分析[J].当代医药论丛,2015,13(3):168.
[3]林洪彬.龙生蛭胶囊治疗气虚血瘀型脑梗死的临床研究[J].中国医药导报,2010,7(19):100.
[4]王巧灵,雷亚贤,姚薇,等.蒸发光散射检测-高效液相色谱法测定龙生蛭胶囊中黄芪甲苷的含量[J].时珍国医国药,2007,18(7):1686.
[5]董乙文,李天雪,褚朝森,等. UPLC-MS/MS法同时定量测定补中益气丸中的15种化合物[J].药物分析杂志,2017,37(7):1228.
[6] Zhang Y C,Xu H Y,Chen X M,et al. Simultaneous quantification of 17 constituents from Yuanhu Zhitong tablet using rapid resolution liquid chromatography coupled with a triple quadrupole electrospray tandem mass spectrometry[J]. J Pharmaceut Biomed,2011,56(3):497.
[7]中国药典.一部[S]. 2015:62.
[8]张冬青,王海宝,王淑芳,等.毛蕊异黄酮生物活性的研究进展[J].中国中药杂志,2015,40(22):4339.
[9]左爱华,王莉,肖红斌.藁本内酯药理学和药代动力学研究进展[J].中国中药杂志,2012,37(22):3350.
[10]张丽娟,刘继勇,姚翀,等.洋川芎内酯类化合物药理作用研究进展[J].中国药学杂志,2015,50(13):1081.
[11]范惠霞.刺五加中主要活性成分的药动学研究[D].济南:济南大学,2014.
[12]郑世存,李晓宇,欧阳兵,等.芍药苷药理作用研究新进展[J].中国药物警戒,2012,9(2):100.
[13]冀兰鑫,黄浩,李长志,等.赤芍药理作用的研究进展[J].药物评价研究,2010,33(3):233.
[14] Wang Q,Song W,Qiao X,et al. Simultaneous quantification of50 bioactive compounds of the traditional Chinese medicine formula Gegen-Qinlian decoction using ultra-high performance liquid chromatography coupled with tandem mass spectrometry[J]. J Chromatogr A,2016,1454:15.
[15]徐澄梅,任浩,钱大玮,等.采用UPLC-TQ-MS同时测定银杏花粉24种资源性化学成分[J].中国中药杂志,2015,40(11):2157.
[16]李震宇,段亚辉,秦雪梅,等.中药质量差异性研究的思考[J].药学学报,2017,52(12):1820.
[17]张伯礼,陈传宏.中药现代化20年(1996—2015)[M].上海:上海科学技术出版社,2016:141.
[18]于玲,王知斌,王秋红,等.黄芪中黄酮类化合物药理作用研究进展[J].中医药信息,2018,35(2):104.
[19]李露,戴婷,李小龙,等.苦杏仁苷药理作用的研究进展[J].吉林医药学院学报,2016,37(1):63.
[20]谭晓斌,贾晓斌,沈明勤,等.刺五加抗脑缺血作用物质基础纯化工艺优选[J].中成药,2008(4):504.
[21]李辰,王晓燕,胡绪玮,等.刺五加抗疲劳活性部位中刺五加苷B的含量测定[J].中国中药杂志,2008,33(23):2800.
[22]董文婷,霍金海,张海燕,等.刺五加叶的药理作用研究进展[J].中国实验方剂学杂志,2015,21(23):220.
[2]杨桂林.联合应用龙生蛭胶囊和阿司匹林治疗短暂性脑缺血发作的效果分析[J].当代医药论丛,2015,13(3):168.
[3]林洪彬.龙生蛭胶囊治疗气虚血瘀型脑梗死的临床研究[J].中国医药导报,2010,7(19):100.
[4]王巧灵,雷亚贤,姚薇,等.蒸发光散射检测-高效液相色谱法测定龙生蛭胶囊中黄芪甲苷的含量[J].时珍国医国药,2007,18(7):1686.
[5]董乙文,李天雪,褚朝森,等. UPLC-MS/MS法同时定量测定补中益气丸中的15种化合物[J].药物分析杂志,2017,37(7):1228.
[6] Zhang Y C,Xu H Y,Chen X M,et al. Simultaneous quantification of 17 constituents from Yuanhu Zhitong tablet using rapid resolution liquid chromatography coupled with a triple quadrupole electrospray tandem mass spectrometry[J]. J Pharmaceut Biomed,2011,56(3):497.
[7]中国药典.一部[S]. 2015:62.
[8]张冬青,王海宝,王淑芳,等.毛蕊异黄酮生物活性的研究进展[J].中国中药杂志,2015,40(22):4339.
[9]左爱华,王莉,肖红斌.藁本内酯药理学和药代动力学研究进展[J].中国中药杂志,2012,37(22):3350.
[10]张丽娟,刘继勇,姚翀,等.洋川芎内酯类化合物药理作用研究进展[J].中国药学杂志,2015,50(13):1081.
[11]范惠霞.刺五加中主要活性成分的药动学研究[D].济南:济南大学,2014.
[12]郑世存,李晓宇,欧阳兵,等.芍药苷药理作用研究新进展[J].中国药物警戒,2012,9(2):100.
[13]冀兰鑫,黄浩,李长志,等.赤芍药理作用的研究进展[J].药物评价研究,2010,33(3):233.
[14] Wang Q,Song W,Qiao X,et al. Simultaneous quantification of50 bioactive compounds of the traditional Chinese medicine formula Gegen-Qinlian decoction using ultra-high performance liquid chromatography coupled with tandem mass spectrometry[J]. J Chromatogr A,2016,1454:15.
[15]徐澄梅,任浩,钱大玮,等.采用UPLC-TQ-MS同时测定银杏花粉24种资源性化学成分[J].中国中药杂志,2015,40(11):2157.
[16]李震宇,段亚辉,秦雪梅,等.中药质量差异性研究的思考[J].药学学报,2017,52(12):1820.
[17]张伯礼,陈传宏.中药现代化20年(1996—2015)[M].上海:上海科学技术出版社,2016:141.
[18]于玲,王知斌,王秋红,等.黄芪中黄酮类化合物药理作用研究进展[J].中医药信息,2018,35(2):104.
[19]李露,戴婷,李小龙,等.苦杏仁苷药理作用的研究进展[J].吉林医药学院学报,2016,37(1):63.
[20]谭晓斌,贾晓斌,沈明勤,等.刺五加抗脑缺血作用物质基础纯化工艺优选[J].中成药,2008(4):504.
[21]李辰,王晓燕,胡绪玮,等.刺五加抗疲劳活性部位中刺五加苷B的含量测定[J].中国中药杂志,2008,33(23):2800.
[22]董文婷,霍金海,张海燕,等.刺五加叶的药理作用研究进展[J].中国实验方剂学杂志,2015,21(23):220.