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高效液相色谱-质谱联用对醒脑注射液化学成分的综合分析

Comprehensive analysis of chemical constituents in Xingxiong injection by high performance liquid chromatography coupled with mass spectrometry.

作者信息

Guo Long, Dou Li-Li, Duan Li, Liu Ke, Bi Zhi-Ming, Li Ping, Liu E-Hu

机构信息

State Key Laboratory of Natural Medicines, China Pharmaceutical University, Nanjing 210009, China.

State Key Laboratory of Natural Medicines, China Pharmaceutical University, Nanjing 210009, China.

出版信息

Chin J Nat Med. 2015 Sep;13(9):711-20. doi: 10.1016/S1875-5364(15)30071-6.

Abstract

Xingxiong injection (XXI) is a widely used Chinese herbal formula prepared by the folium ginkgo extract and ligustrazine for the treatment of cardiovascular and cerebrovascular diseases. Compared with the pharmacological studies, chemical analysis and quality control studies on this formula are relatively limited. In the present study, a high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS) method was applied to comprehensive analysis of constituents in XXI. According to the fragmentation rules and previous reports, thirty ginkgo flavonoids, four ginkgo terpene lactones, and one alkaloid were identified. A high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ MS) method was then applied to quantify ten major constituents in XXI. The method validation results indicated that the developed method had desirable specificity, linearity, precision and accuracy. The total contents of ginkgo flavonoids were about 22.05-25.51 μg·mL(-1) and the ginkgo terpene lactones amounts were about 4.41-8.70 μg·mL(-1) in six batches of XXI samples, respectively. Furthermore, cosine ratio algorithm and distance measurements were employed to evaluate the similarity of XXI samples, and the results demonstrated a high-quality consistency. This work could provide comprehensive information on the quality control of Xingxiong injection, which be helpful in the establishment of a rational quality control standard.

摘要

杏芎注射液(XXI)是一种广泛应用的中药复方制剂,由银杏叶提取物和川芎嗪制成,用于治疗心脑血管疾病。与该复方制剂的药理研究相比,其化学分析和质量控制研究相对有限。在本研究中,采用高效液相色谱-四极杆飞行时间质谱联用(HPLC-QTOF MS)方法对杏芎注射液中的成分进行全面分析。根据裂解规律和既往报道,鉴定出30种银杏黄酮类化合物、4种银杏萜内酯和1种生物碱。随后采用高效液相色谱-三重四极杆质谱联用(HPLC-QQQ MS)方法对杏芎注射液中的10种主要成分进行定量分析。方法学验证结果表明,所建立的方法具有良好的专属性、线性、精密度和准确度。6批杏芎注射液样品中银杏黄酮类化合物的总含量分别约为22.05 - 25.51 μg·mL(-1),银杏萜内酯的含量分别约为4.41 - 8.70 μg·mL(-1)。此外,采用余弦比算法和距离测量法对杏芎注射液样品的相似度进行评价,结果显示其具有较高的质量一致性。本研究可为杏芎注射液的质量控制提供全面信息,有助于建立合理的质量控制标准。

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