心脑脉舒口服液质量标准提高及工艺优化
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摘要
目的提高心脑脉舒口服液质量控制标准,及其制剂工艺优化。方法采用Sepax HP-C18 (250mm×4.6 mm,5μm);流动相:甲醇(A)-0.2%乙酸水(B)=30∶70;流速:1.0 ml/min;检测波长:403 nm;柱温:25℃;进样量:10μl,对心脑脉舒口服液中羟基红花黄色素A含量进行测定。以羟基红花黄色素A含量为指标,采用单因素考察的方法对心脑脉舒口服液制剂工艺进行优化。结果羟基红花黄色素A在0.04～0.20μg内呈良好的线性关系(r=0.999 8),平均回收率为98.48%,RSD=1.39%。优化提取工艺为水浸提24 h,浓缩0.5 h,浓缩液利用2.5倍量的40%乙醇进行醇沉,药液应调节至pH为5.5。结论新建心脑脉舒口服液质量控制方法简单、重现性良好、准确可靠,可用于心脑脉舒口服液质量控制质量评价。优化后的制剂工艺有效成分损失最少,并尽量保留了该处方中的有效成分。
Objective To improve the quality control standard of Xinnao Maishu oral Solution, and optimize its preparation process. Methods The content of Safflomin A in the Xinnao Maishu oral solution is determined on a Sepax HP-C18(250 mm × 4.6 mm, 5 μm) with methyl alcohol and 0.2 % acetic acid(30 : 70) as the mobile phase. The flow rate is 1.0 ml/min. The detection wavelength is 260 nm, and the column temperature is 25℃. The injection volume is 10 μl. With the content of Safflomin A as the indicator, and the method of single factor investigation is used to optimize the preparation process of the oral solution. Results The linear range of Safflomin A is 0.04 ～ 0.20 μg(r = 0.999 8) which indicated the linearity of this method is all right. The average recovery of them are 98.48 % and the RSD = 1.39 %. The optimized extraction process is water leaching of 24 h, concentrated 0.5 h, and the concentrated liquid is used to make alcohol sink with a 40 % ethanol of 2.5 times.The liquid should be adjusted to pH 5.5. Conclusion The new quality control method is simple, reproducible and accurate, and can be used to evaluate the quality control of Xinnao Maishu oral Solution. The optimized preparation process has the least loss of effective components, and the effective components in the prescription are kept as far as possible.
Objective To improve the quality control standard of Xinnao Maishu oral Solution, and optimize its preparation process. Methods The content of Safflomin A in the Xinnao Maishu oral solution is determined on a Sepax HP-C18(250 mm × 4.6 mm, 5 μm) with methyl alcohol and 0.2 % acetic acid(30 : 70) as the mobile phase. The flow rate is 1.0 ml/min. The detection wavelength is 260 nm, and the column temperature is 25℃. The injection volume is 10 μl. With the content of Safflomin A as the indicator, and the method of single factor investigation is used to optimize the preparation process of the oral solution. Results The linear range of Safflomin A is 0.04 ～ 0.20 μg(r = 0.999 8) which indicated the linearity of this method is all right. The average recovery of them are 98.48 % and the RSD = 1.39 %. The optimized extraction process is water leaching of 24 h, concentrated 0.5 h, and the concentrated liquid is used to make alcohol sink with a 40 % ethanol of 2.5 times.The liquid should be adjusted to pH 5.5. Conclusion The new quality control method is simple, reproducible and accurate, and can be used to evaluate the quality control of Xinnao Maishu oral Solution. The optimized preparation process has the least loss of effective components, and the effective components in the prescription are kept as far as possible.
引文
[1]党大胜,安晔,刘喜凤,等.心脑脉舒口服液治疗冠心病心绞痛的临床疗效观察[J].中国现代应用药学,2014, 31(2):237-240.
[2]姚东,胡北,高军,等.心脑脉舒口服液质量控制与降血脂作用相关研究[J].世界中医药, 2015(11):1774-1776.
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[5]郭涛,戴京美. HPLC法测定心脑脉舒口服液中阿魏酸含量[J].药学实践杂志, 1995(4):225-228.
[6]何进,冯夏,周晓宇,等.心脑脉舒口服液微生物限度检查的方法验证[J].药学服务与研究, 2009, 9(1):71-72.
[7]雷志丹,雷志钧,夏新华,等. HPLC测定红花中羟基红花黄色素A的含量[J].中国当代医药, 2011, 18(7):45-46.
[8]姚苗苗,任爱农,董仲才. RP-HPLC法同时测定红花中羟基红花黄色素A与红花黄色素A的含量[J].药物分析杂志, 2010(2):263-265.
[9]牛凯,张宇,郑为超.羟基红花黄色素A与心血管作用研究进展[J].辽宁中医药大学学报, 2012(12):70-72.
[10]江维,宋宏安,孙代华,等.红花注射液制备工艺探讨[J].中国药师,2013, 16(10):1544-1547.
[2]姚东,胡北,高军,等.心脑脉舒口服液质量控制与降血脂作用相关研究[J].世界中医药, 2015(11):1774-1776.
[3]国家药典委员会.中华人民共和国药典[S].北京:中国医药科技出版社,2015:151.
[4]宋洪涛,郭涛,迟卫国,等.超滤法制备心脑脉舒口服液及临床疗效观察[J].药学实践杂志, 1993(4):45-46.
[5]郭涛,戴京美. HPLC法测定心脑脉舒口服液中阿魏酸含量[J].药学实践杂志, 1995(4):225-228.
[6]何进,冯夏,周晓宇,等.心脑脉舒口服液微生物限度检查的方法验证[J].药学服务与研究, 2009, 9(1):71-72.
[7]雷志丹,雷志钧,夏新华,等. HPLC测定红花中羟基红花黄色素A的含量[J].中国当代医药, 2011, 18(7):45-46.
[8]姚苗苗,任爱农,董仲才. RP-HPLC法同时测定红花中羟基红花黄色素A与红花黄色素A的含量[J].药物分析杂志, 2010(2):263-265.
[9]牛凯,张宇,郑为超.羟基红花黄色素A与心血管作用研究进展[J].辽宁中医药大学学报, 2012(12):70-72.
[10]江维,宋宏安,孙代华,等.红花注射液制备工艺探讨[J].中国药师,2013, 16(10):1544-1547.