| 王峰,聂黎行,于健东,戴忠,马双成.活血止痛制剂中三七的专属性鉴别方法研究[J].中国药事,2019,33(7):760-766 |
| 活血止痛制剂中三七的专属性鉴别方法研究 |
| Study on Specific Identification Method of Notoginseng Radix et Rhizoma in Huoxue Zhitong Preparations |
| 投稿时间：2019-02-09 |
| DOI：10.16153/j.1002-7777.2019.07.007 |
| 中文关键词: 活血止痛散 活血止痛胶囊 三七 专属性鉴别 高效薄层色谱法 高分离度快速液相色谱-三重串联四极杆质谱 人参 红参 三七茎叶 |
| 英文关键词: Huoxue Zhitong Powders Huoxue Zhitong Capsules Notoginseng Radix et Rhizoma specific identification high performance thin layer chromatography (HPTLC) rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry (RRLC-QQQ/MS) Ginseng Radix et Rhizoma Ginseng Radix et Rhizoma Rubra Notoginseng Caulis et Folium |
| 基金项目:国家自然科学基金（编号81303194）；中国食品药品检定研究院学科带头人培养基金（编号2017X1） |
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| 中文摘要: |
| 目的：建立活血止痛散和活血止痛胶囊中三七的专属性鉴别方法，并采用高分离度快速液相色谱-三重串联四极杆质谱（RRLC-QQQ/MS）对结果加以验证。方法：采用高效薄层色谱法研究三七与其混伪品人参、红参、三七茎叶的特征条带。以高效硅胶G薄层板为固定相，二氯甲烷-无水乙醇-水（70：45：6.5）展开，10%硫酸乙醇溶液显色，105℃加热至条带清晰。分别置紫外光灯（365 nm）和日光下检视。RRLC-QQQ/MS分析采用Agilent Rapid Resolution HT SB-C18（2.1 mm×100 mm，1.8 μm）色谱柱，以5 mmol·L-1醋酸铵溶液-乙腈为流动相梯度洗脱。离子化模式为ESI-，碎裂电压100 V。结果：三七可检出三七皂苷R1，未检出人参皂苷Rb3、人参皂苷Rf。人参和红参可检出人参皂苷Rb3和人参皂苷Rf，未检出三七皂苷R1。三七茎叶可检出人参皂苷Rb3，未检出三七皂苷R1或人参皂苷Rg1。以三七对照药材、三七皂苷R1（应检出）和人参皂苷Rb3（不得检出）为对照，可实现活血止痛制剂中三七的专属性鉴别和人参（红参）或三七茎叶的非法掺杂投料检查。6个厂家的93批样品均未发现人参、红参或三七茎叶冒充三七非法投料。RRLC-QQQ/MS与高效薄层分析结果一致。结论：该方法简便、快速、灵敏、准确，可为含三七中成药的质量控制提供参考。 |
| 英文摘要: |
| Objective:To establish specific identification method of Notoginseng Radix et Rhizoma in Huoxue Zhitong Powders and Huoxue Zhitong Capsules and validate the results by rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry (RRLC-QQQ/MS). Methods:High performance thin layer chromatography (HPTLC) was used to study the characteristic bands of Notoginseng Radix et Rhizoma and its adulterants, such as Ginseng Radix et Rhizoma, Ginseng Radix et Rhizoma Rubra and Notoginseng Caulis et Folium. High performance silica gel G was used as the coating substance and a mixture of dichloromethane, anhydrous ethanol and water (70:45:6.5) was used as the mobile phase. 10% solution of sulfuric acid in ethanol was sprayed and the plate was heated at 105℃ until the bands were distinct. The plates were examined in daylight and under ultraviolet light at 365 nm. The RRLC-QQQ/MS analysis was performed on an Agilent Rapid Resolution HT SB-C18 (2.1 mm×100 mm, 1.8 μm) column. The mobile phase was composed of acetonitrile and 5 mmol·L-1 ammonium acetate with grade elution. Ionization mode was ESI-and ragmentation voltage was 100 V. Results:Notoginsenoside R1 was detected in Notoginseng Radix et Rhizoma while ginsenoside Rb3 or ginsenoside Rf was not detected. Ginsenoside Rb3 and ginsenoside Rf were detected in Ginseng Radix et Rhizoma and Ginseng Radix et Rhizoma Rubra while Notoginsenoside R1 was not detected. Ginsenoside Rb 3 was detected in Notoginseng Caulis et Folium while notoginsenoside R1 or ginsenoside Rg1 was not detected. Using Notoginseng Radix et Rhizoma as reference medicinal material, notoginsenoside R1 reference substance (should be detected) and ginsenoside Rb3 reference substance (should not be detected) as references, specific identification of Notoginseng Radix et Rhizoma and test of illegal adulteration of Ginseng Radix et Rhizoma, Ginseng Radix et Rhizoma Rubra or Notoginseng Caulis et Folium in Huoxue Zhitong Preparations could be achieved. Illegal adulteration of Ginseng Radix et Rhizoma, Ginseng Radix et Rhizoma Rubra or Notoginseng Caulis et Folium was not found in 93 batches of samples from 6 manufactures. Results of RRLCQQQ/MS were consistent with those of HPTLC. Conclusion:The established method is simple, fast, sensitive, accurate and can provide references for quality control of Chinese patent medicines containing Notoginseng Radix et Rhizoma. |
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