抗痨清肺颗粒HPLC特征图谱及液质联用剖析.docVIP

抗痨清肺颗粒HPLC特征图谱及液质联用剖析 　　摘要：目的 建立抗痨清肺颗粒高效液相色谱（HPLC）特征图谱。方法 采用Kromasil C18色谱柱（4.6 mm×250 mm，5 μm），以乙腈-1%醋酸水溶液为流动相进行梯度洗脱（0～50 min，5%→15%乙腈；50～70 min，15%→25%乙腈；70～80 min，25%→40%乙腈；80～90 min，40%→65%乙腈；90～120 min，65%→95%乙腈），流速1.0 mL/min，检测波长290 nm，柱温30 ℃；采用液质联用（HPLC-MS/MS）技术进行色谱峰组分的鉴定。结果 10批样品相似度均0.995，确立了13个共有特征峰，对其中10个共有峰进行了来源归属，对其中8个共有峰进行了成分鉴别。结论 建立的HPLC特征图谱可用于抗痨清肺颗粒的质量控制。 　　关键词：抗痨清肺颗粒；特征图谱；高效液相色谱法；液质联用 　　DOI：10.3969/j.issn.1005-5304.2015.08.024 　　中图分类号：R284.1 文献标识码：A 文章编号：1005-5304（2015）08-0088-04 　　HPLC Characteristic Chromatogram and HPLC-MS/MS Analysis of Kanglao Qingfei Granules TANG Lin1， LUO Chun-qing1， XIA Xin-hua1， ZENG Jian-guo2， LIU Yan-ke2 （1.School of Pharmacy， Hunan University of Chinese Medicine， Changsha 410208， China；2.Changsha Central Hospital， Changsha 410004， China） 　　Abstract：Objective To establish HPLC characteristic chromatogram of Kanglao Qingfei Granules. Methods HPLC analysis of samples was performed on Kromasil C18 column （4.6 mm × 250 mm， 5 μm）， with acetonitrile-1% glacial acetic acid as the mobile phase of gradient elution （0-50 min， 5%→15% acetonitrile；50-70 min， 15%→25% acetonitrile；70-80 min， 25%→40% acetonitrile；80-90 min， 40%→65% acetonitrile， 90-120 min， 65%→95% acetonitrile）；the volume flow rate was 1.0 mL/min；detection wavelength was set at 290 nm；column temperature was 30 ℃. Chromatographic peaks were identified by HPLC-MS/MS method. Results The similarity degrees of 10 batches of samples were all greater than 0.995， and 13 chromatographic peaks were determined as common characteristic peaks， of which 10 peaks were confirmed in the source attribution and 8 peaks were identified in chemical component. Conclusion The established HPLC characteristic chromatogram can be used for the quality control of Kanglao Qingfei Granules. 　　Key words：Kanglao Qingfei Granules；characteristic chromatogram；HPLC；HPLC-MS/MS 　　抗痨清肺颗粒由百部、橘络、矮地茶、黄精、玉竹等7味药组成，源于长沙市中心医院的临床经验方，主要用于多耐药性肺结核的治疗。该制剂成分复杂，其中玉竹、黄精等含有较多皂苷及多糖类成分[1-2]，橘络、矮地茶等含有较多黄酮类、香豆素类等成分[3-