Direct and comprehensive analysis of ginsenosides and diterpene alkaloids in Shenfu injection by combinatory liquid chromatography-mass spectrometric techniques
Direct and comprehensive analysis of ginsenosides and diterpene alkaloids in Shenfu injection by combinatory liquid chromatography-mass spectrometric techniques
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DOI：
10.1016/j.jpba.2013.12.041
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发表时间：
2014-04-15
影响因子：
3.4
通讯作者：
Li, Ping
中科院分区：
文献类型：
--
作者：
Yang, Hua;Liu, Lei;Li, Ping
参附注射液（SFI）是一种广泛使用的治疗心脏病的中药制剂，由红参和加工附子根制成。 SFI 的临床观察和药理作用已得到充分研究。然而，该制剂的化学分析和质量控制研究相对有限，特别是关于有毒附子生物碱。本工作采用高效液相色谱-四极杆飞行时间质谱(HPLC-QTOF MS)方法对SFI中的成分进行综合分析。高灵敏度 MS 可以直接分析进样，无需额外的样品预处理。利用诊断离子和裂解规则，我们在 SFI 中鉴定出了 23 种痕量二萜生物碱、19 种人参皂苷、1 种人参三醇和 1 种 5-羟甲基糠醛。然后使用带有选择离子监测的 LC-MS 方法对 24 种主要生物碱和人参皂苷进行定量。该方法在线性、准确度和精密度方面得到验证。特别是，二萜生物碱的定量限低至 0.4-18 ng/mL。 5批SFI样品中皂苷和生物碱的总浓度分别约为676-742μg/mL和3-7μg/mL。最后，引入余弦比和欧几里德距离来评估SFI样品的批次间重现性，结果表现出较高的质量一致性。基于 LC-MS 的复杂成分的全局识别和定量有望在草药产品的质量控制和批量监控中得到广泛应用。 (C) 2014 Elsevier B.V. 保留所有权利。
Shenfu injection (SFI) is a widely used Chinese herbal formulation for cardiac diseases prepared from red ginseng and processed aconite root. Clinical observations and pharmacological effects on SFI have been well investigated. Chemical analysis and quality control studies of this formulation, however, are relatively limited, especially regarding toxic aconite alkaloids. In this work, 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 SFI. Highly sensitive MS allows direct analysis of injections without additional sample pretreatment required. Using diagnostic ions and fragmentation rules, we identified 23 trace diterpene alkaloids, nineteen ginseng saponins, one panaxytriol, and one 5-hydroxymethylfurfural in SFI. A LC-MS method with selected ion monitoring was then used to quantify 24 major alkaloids and ginsenosides. The method was validated in terms of linearity, accuracy and precision. Especially, the limits of quantification were low to 0.4-18 ng/mL for diterpene alkaloids. The total concentrations of saponins and alkaloids were about 676-742 mu g/mL and 3-7 mu g/mL in five batches of SFI samples, respectively. Finally, cosine ratio and euclidean distance were introduced to evaluate the batch-to-batch reproducibility of SFI samples, and the results demonstrated high quality consistency. Global identification and quantification of complex constituents based on LC-MS promises wide applications in quality control and batch monitoring for herbal products. (C) 2014 Elsevier B.V. All rights reserved.