连栀矾溶液HPLC指纹图谱研究
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摘要
目的:建立中药复方制剂连栀矾溶液的HPLC指纹图谱,为该制剂的质量控制提供参考。方法:采用Phenomenex luna C_(18)色谱柱(250 mm×4. 6 mm,5μm),以0. 1%三乙胺0. 2%磷酸水溶液-甲醇-乙腈为流动相进行梯度洗脱,流速为1. 0 ml·min~(-1),检测波长为230 nm,柱温为30℃,建立连栀矾溶液HPLC指纹图谱,运用"中药色谱指纹图谱相似度评价系统"(2012版)软件对10批制剂进行相似度评价,通过对照品保留时间及光谱图的比对,对连栀矾溶液中4种化学成分进行指认,通过连栀矾溶液组方单味药和复方的HPLC比较,初步分析复方中化学成分的来源和归属。结果:建立的连栀矾溶液HPLC指纹图谱专属性、精密度、重复性和稳定性均良好; 10批连栀矾溶液指纹图谱与对照指纹图谱相似度值在0. 994～1. 000,相似度良好;与组方单位药材对比,连栀矾溶液指纹图谱中大部分色谱峰来源于黄连。结论:建立的连栀矾溶液HPLC指纹图谱能全面反映连栀矾溶液中多组分的整体特征,可用于连栀矾溶液的质量控制。
Objective: To establish an HPLC fingerprint of Lianzhifan solution to provide reference for the effective quality control.Methods: The HPLC separation was performed on a Phenomenex luna C_(18) (250 mm × 4. 6 mm,5 μm) column with the mobile phase consisting of water (0. 1% triethylamine and 0. 2% phosphoric acid)-methanol-acetonitrile with gradient elution at the flow rate of 1. 0ml·min~(-1). The detection wavelength was set at 230 nm and the column temperature was 30℃. Ten batches of Lianzhifan solution were collected to assess the similarities,the main peaks in the fingerprint were identified by comparing the retention time with that of the reference substances,and the source and attribution of chemical components in the preparation were analyzed by comparing with that in the single herb. Results: The established fingerprint of Lianzhifan solution was specific,precise and stable. Compared with the reference fingerprint,the fingerprint similarities of the 10 batches of Lianzhifan solution were between 0. 994 and 1. 000. A comparative analysis showed that most of the chromatographic peaks in the fingerprint of Lianzhifan solution were derived from Coptis. Conclusion:The analytical method of HPLC fingerprint can reflect overall characteristics of multicomponent and provide evidence for the quality control of Lianzhifan solution.
Objective: To establish an HPLC fingerprint of Lianzhifan solution to provide reference for the effective quality control.Methods: The HPLC separation was performed on a Phenomenex luna C_(18) (250 mm × 4. 6 mm,5 μm) column with the mobile phase consisting of water (0. 1% triethylamine and 0. 2% phosphoric acid)-methanol-acetonitrile with gradient elution at the flow rate of 1. 0ml·min~(-1). The detection wavelength was set at 230 nm and the column temperature was 30℃. Ten batches of Lianzhifan solution were collected to assess the similarities,the main peaks in the fingerprint were identified by comparing the retention time with that of the reference substances,and the source and attribution of chemical components in the preparation were analyzed by comparing with that in the single herb. Results: The established fingerprint of Lianzhifan solution was specific,precise and stable. Compared with the reference fingerprint,the fingerprint similarities of the 10 batches of Lianzhifan solution were between 0. 994 and 1. 000. A comparative analysis showed that most of the chromatographic peaks in the fingerprint of Lianzhifan solution were derived from Coptis. Conclusion:The analytical method of HPLC fingerprint can reflect overall characteristics of multicomponent and provide evidence for the quality control of Lianzhifan solution.
引文
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11毛爱丽.HPLC法测定黄连上清片中4种成分的含量[J].中国药师,2016,19(1):196-197,201
12席桂同,陈述.复方黄连素片中盐酸小檗碱含量测定[J].世界中医药,2015,10(2):252-254,257
13李翔,刘皈阳,马建丽,等.HPLC法测定丹膝颗粒中栀子苷的含量[J].中国药师,2013,16(3):468-469
14吴红娟,王清波,谭朝阳,等.不同来源栀子中栀子苷含量测定[J].湖南中医药大学学报,2010,30(5):35-37
2马丽丽.连栀矾溶液加锡类散保留灌肠治疗慢性溃疡性直肠炎疗效观察[J].西北药学杂志,2013,28(4):416-417
3余腾江,杨向东,理习阳.连栀矾溶液联合康复新液对41例肛漏术后换药的疗效观察[J].云南中医中药杂志,2014,35(1):45-464袁学刚,王战国,胡慧玲,等.HPLC测定连栀矾溶液中表小檗碱、黄连碱、巴马汀和盐酸小檗碱的含量[J].中药与临床,2016,7(1):31-33
5刘东方,赵丽娜,李银峰,等.中药指纹图谱技术的研究进展及应用[J].中草药,2016,47(22):4085-4094
6刁嘉茵,徐灿,王淑美,等.中药指纹图谱与药效相关性研究进展[J].药学研究,2018,37(3):165-168
7杨静,罗廷顺.清火栀麦片HPLC指纹图谱的建立和3种成分含量测定[J].中国药师,2017,20(4):673-676,679
8周忆新,钟水生.黄连上清胶囊中栀子苷的含量测定[J].抗感染药学,2017,14(5):915-917
9韩建国,孙占文,余卫兵.HPLC法测定牛黄上清丸中栀子苷的含量[J].中国药师,2012,15(11):1653-1654
10刘芳,张浩,青琳森.黄连HPLC数字化指纹图谱研究及7种生物碱含量测定[J].中国中药杂志,2013,38(21):3713-3719
11毛爱丽.HPLC法测定黄连上清片中4种成分的含量[J].中国药师,2016,19(1):196-197,201
12席桂同,陈述.复方黄连素片中盐酸小檗碱含量测定[J].世界中医药,2015,10(2):252-254,257
13李翔,刘皈阳,马建丽,等.HPLC法测定丹膝颗粒中栀子苷的含量[J].中国药师,2013,16(3):468-469
14吴红娟,王清波,谭朝阳,等.不同来源栀子中栀子苷含量测定[J].湖南中医药大学学报,2010,30(5):35-37