| 高效液相-高分辨飞行时间质谱对复方夏枯草消瘤方化学成分的鉴别 |
| 投稿时间：2019-07-25 修订日期：2019-11-12 点此下载全文 |
| 引用本文：戴媛媛,汪晓河,马明华,计强国,顾小燕,吴铁军,年华.高效液相-高分辨飞行时间质谱对复方夏枯草消瘤方化学成分的鉴别[J].药学实践杂志,2020,38(2):138~142,155 |
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| 基金项目:上海市卫生和计划生育委员会科研项目（201440386）；上海中医药大学高峰高原学科项目（KY111.20.81）；上海市科学技术委员会科研计划项目（16401902100） |
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| 中文摘要:目的 应用高效液相-高分辨飞行时间质谱（HPLC-TOF/MS）技术鉴别夏枯草消瘤方的化学成分。方法 色谱分离采用ACE（3.0 mm×150 mm）色谱柱；流动相为甲醇(A)和0.1%甲酸水(B)，梯度洗脱：0~5 min：5%A，5~10 min：5%~15%A，10~30 min：15%~45%A，30~40 min：45%~70%B，40~50 min：70%~90%B；进样量2 μl，流速为0.4 ml/min；柱温为25 ℃。质谱定性采用飞行时间质谱，采用ESI离子源，正、负离子模式共同监测，参比离子m/z 121.9856，1033.9881；扫描范围m/z 100-1200。结果 共鉴别出夏枯草消瘤方中37种化学成分，正离子模式碎片电压160 V条件下8个；负离子模式碎片电压160 V条件下28个，碎片电压260 V条件下19个；正负离子均有响应4个，负离子模式两种碎片电压下均有响应16个，并对成分进行了药材归属。结论 建立了一种基于HPLC-TOF/MS技术对夏枯草消瘤方的化学成分进行鉴别的有效方法，为其质量控制及体内的深入研究奠定了基础。 |
| 中文关键词:夏枯草消瘤方 化学成分 鉴别 高效液相-高分辨飞行时间质谱 |
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| Identification of chemical constituents of Xiakucao Xiaoliu mixture by HPLC-TOF/MS |
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| Abstract:Objective To identify the chemical constituents of Xiakucao Xiaoliu mixture by high performance liquid chromatography-high resolution time-of-flight mass spectrometry (HPLC-TOF/MS).Methods The chromatographic separation ACE (3.0mm×150 mm) column was used. The mobile phase was methanol (A) and 0.1% formic acid (B). The gradient elution was: 0-5 min, 5% A; 5-10 min, 5%-15% A; 10-30 min, 15%-45%A; 30-40 min, 45%-70%B; 40-50 min, 70%-90%B. The injection volume was 2 μl. The flow rate was 0.4 ml/min. The column temperature was 25℃. The mass spectrometry was characterized by time-of-flight mass spectrometry, using ESI ion source. The common monitoring was in positive and negative ion mode. The reference ion was m/z 121.9856, 1033.9881. The scanning range was m/z 100-1200.Results A total of 37 chemical constituents were identified in the Xiakucao Xiaoliu mixture, 8 in the positive ion mode fragment voltage of 160 V, 28 in the negative ion mode fragment voltage of 160 V, and 19 in the fragment voltage of 260 V. Both positive and negative ions had 4 responses. The negative ion mode has 16 responses under both fragment voltages. And the ingredients were medicinal.Conclusion An effective method for the identification of the chemical constituents of Prunella vulgaris L. by HPLC-TOF/MS was established, which laid a foundation for its quality control and in-depth study in vivo. |
| keywords:Xiakucao Xiaoliu mixture chemical composition identification high performance liquid-high resolution time-of-flight mass spectrometry |
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