HPLC波长切换法在活血止痛胶囊质量评价中的应用
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摘要
目的:基于HPLC波长切换技术评价活血止痛胶囊中当归和乳香的质量。建立松香酸的检查方法,同时测定阿魏酸和11-羰基-β-乙酰乳香酸的含量。方法:色谱柱:Agilent TC-C_(18)(250 mm×4. 6 mm,5μm);柱温30℃;流动相:乙腈-0. 1%甲酸梯度洗脱(0～8 min:30%乙腈; 8～10 min:30%～80%乙腈; 10～30 min:80%乙腈; 30～40 min:30%乙腈);流速1. 0 mL·min~(-1);阿魏酸检测波长:321 nm;松香酸检测波长:240 nm; 11-羰基-β-乙酰乳香酸检测波长:250 nm。结果:松香酸检出限为3. 13 ng·mL~(-1)。阿魏酸和11-羰基-β-乙酰乳香酸分别在0. 01～100μg·mL~(-1)和0. 2～200μg·mL~(-1)范围内线性关系良好,平均回收率分别为99. 8%和102. 6%。3个厂家的9批样品阿魏酸含量在0. 20～0. 30 mg·g~(-1)之间,11-羰基-β-乙酰乳香酸含量在1. 96～3. 91 mg·g~(-1)之间。结论:所建方法准确、快速、简便,可为活血止痛胶囊的质量标准提高提供实验基础。
Objective: To evaluate the quality of Angelicae Sinensis Radix and Olibanum in Huoxue Zhitong capsules based on high performance liquid chromatography (HPLC) combined with wavelength switching.The testing method for abietic acid was established and the contents of ferulic acid and acetyl-11-keto-β-boswellic acid were determined simultaneously. Methods: The separation was performed on an Agilent TC-C_(18) (250 mm ×4. 6 mm,5 μm) column and the column temperature was set at 30 ℃. The mobile phase was composed of acetonitrile and 0. 1% formic acid with gradient elution (0 ～ 8 min: 30% acetonitrile; 8 ～ 10 min: 30% ～ 80% acetonitrile;10 ～ 30 min: 80% acetonitrile) at a current speed of 1. 0 mL·min~(-1). The detection wavelengths were set at 321 nm for ferulic acid,240 nm for abietic acid and 250 nm for acetyl-11-keto-β-boswellic acid,respectively. Results:The limit of detection of abietic acid was 3. 13 ng·mL~(-1). The calibration curves of ferulic acid and acetyl-11-keto-β-boswellic acid showed good linearity within the ranges of 0.01 ～100 μg·mL~(-1) and 0. 2 ～ 200 μg·mL~(-1),respectively.And the average recoveries for the above analytes were 99. 8% and 102. 6%,respectively. The contents of ferulic acid and acetyl-11-keto-β-boswellic acid in 9 batches of samples from 3 manufactures were within 0. 20 ～ 0. 30 mg·g~(-1) and 1. 96 ～ 3. 91 mg·g~(-1),respectively. Conclusion: The proposed method is accurate,rapid and simple,whichprovides scientific basis for improvement of the quality standard of Huoxue Zhitong capsules.
Objective: To evaluate the quality of Angelicae Sinensis Radix and Olibanum in Huoxue Zhitong capsules based on high performance liquid chromatography (HPLC) combined with wavelength switching.The testing method for abietic acid was established and the contents of ferulic acid and acetyl-11-keto-β-boswellic acid were determined simultaneously. Methods: The separation was performed on an Agilent TC-C_(18) (250 mm ×4. 6 mm,5 μm) column and the column temperature was set at 30 ℃. The mobile phase was composed of acetonitrile and 0. 1% formic acid with gradient elution (0 ～ 8 min: 30% acetonitrile; 8 ～ 10 min: 30% ～ 80% acetonitrile;10 ～ 30 min: 80% acetonitrile) at a current speed of 1. 0 mL·min~(-1). The detection wavelengths were set at 321 nm for ferulic acid,240 nm for abietic acid and 250 nm for acetyl-11-keto-β-boswellic acid,respectively. Results:The limit of detection of abietic acid was 3. 13 ng·mL~(-1). The calibration curves of ferulic acid and acetyl-11-keto-β-boswellic acid showed good linearity within the ranges of 0.01 ～100 μg·mL~(-1) and 0. 2 ～ 200 μg·mL~(-1),respectively.And the average recoveries for the above analytes were 99. 8% and 102. 6%,respectively. The contents of ferulic acid and acetyl-11-keto-β-boswellic acid in 9 batches of samples from 3 manufactures were within 0. 20 ～ 0. 30 mg·g~(-1) and 1. 96 ～ 3. 91 mg·g~(-1),respectively. Conclusion: The proposed method is accurate,rapid and simple,whichprovides scientific basis for improvement of the quality standard of Huoxue Zhitong capsules.
引文
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[5]王瑞忠,何轶,张聿梅,等.西黄丸中11-羰基-β-乙酰乳香酸含量测定及松香酸检查方法研究[J].中国药事,2013,27(4):389-393.
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[8]刘畅,刘玉强,张振秋,等. HPLC波长切换法同时测定山楂丹参分胶囊片中6个指标性成分的含量[J].中国新药杂志,2014,23(3):333-337.
[9]席艳. HPLC梯度洗脱联合波长切换法测定龟鹿补肾胶囊中7种成分的含量[J].沈阳药科大学学报,2018,35(3):207-212.
[10]张毅,周慧.基于HPLC波长切换联合梯度洗脱技术的双参龙胶囊中10种主要成分定量研究[J].中草药,2018,49(5):1081-1086.
[11]王信,李彩东,潘新波,等.基于波长切换技术建立加味小柴胡胶囊质量标准[J].中国药师,2016,19(8):1597-1599.
[12]聂黎行,刘燕,鲁静,等.活血止痛制剂质量评价与研究[J].中国药学杂志,2015,50(2):131-139.
[13]慈小燕,夏媛媛,曾勇,等.应用MDCK-MDR1细胞模型研究3-乙酰基-11-羰基-b-乙酰乳香酸经血脑屏障的通透性[J].中国新药杂志,2013,22(10):1125-1129.
[14]王淳,夏磊,宋志前,等.乳香中5种乳香酸成分含量分析[J].中国中药杂志,2011,36(10):1330-1333.
[15]孙磊,刘丽娜,金红宇,等.乳香、制乳香含量测定研究[J].中国药事,2010,24(10):972-974.
[2]刘昌孝,陈士林,肖小河,等.中药质量标志物(Q-Marker):中药产品质量控制的新概念[J].中草药,2016,4(79):1443-1457.
[3]孙磊,刘燕,逄瑜,等.西黄丸和活血止痛胶囊中乳香及非法添加松香的薄层色谱鉴别[J].中国药事,2013,27(7):722-724.
[4]张亚双,闵春艳.沉香、乳香和没药中非法添加松香酸的研究与讨论[J].西北药学杂志,2013,28(2):133-136.
[5]王瑞忠,何轶,张聿梅,等.西黄丸中11-羰基-β-乙酰乳香酸含量测定及松香酸检查方法研究[J].中国药事,2013,27(4):389-393.
[6]马逢时,李家明.阿魏酸及其衍生物的合成及药效研究进展[J].亚太传统医药,2008,4(5):55-57.
[7]朱志会,李玉文,尚沛津,等.β-乳香酸对血瘀证大鼠血液流变学和血管内皮功能的影响[J].现代生物医学进展,2017,17(20):3806-3810.
[8]刘畅,刘玉强,张振秋,等. HPLC波长切换法同时测定山楂丹参分胶囊片中6个指标性成分的含量[J].中国新药杂志,2014,23(3):333-337.
[9]席艳. HPLC梯度洗脱联合波长切换法测定龟鹿补肾胶囊中7种成分的含量[J].沈阳药科大学学报,2018,35(3):207-212.
[10]张毅,周慧.基于HPLC波长切换联合梯度洗脱技术的双参龙胶囊中10种主要成分定量研究[J].中草药,2018,49(5):1081-1086.
[11]王信,李彩东,潘新波,等.基于波长切换技术建立加味小柴胡胶囊质量标准[J].中国药师,2016,19(8):1597-1599.
[12]聂黎行,刘燕,鲁静,等.活血止痛制剂质量评价与研究[J].中国药学杂志,2015,50(2):131-139.
[13]慈小燕,夏媛媛,曾勇,等.应用MDCK-MDR1细胞模型研究3-乙酰基-11-羰基-b-乙酰乳香酸经血脑屏障的通透性[J].中国新药杂志,2013,22(10):1125-1129.
[14]王淳,夏磊,宋志前,等.乳香中5种乳香酸成分含量分析[J].中国中药杂志,2011,36(10):1330-1333.
[15]孙磊,刘丽娜,金红宇,等.乳香、制乳香含量测定研究[J].中国药事,2010,24(10):972-974.