| 殷世宁,卢京光,宿曼筠,袁航,尹丽华,吴爱英.感冒清热颗粒中藏柴胡检查方法的研究[J].中国药事,2023,(4):461-468 |
| 感冒清热颗粒中藏柴胡检查方法的研究 |
| Study on the Inspection Method of Bupleurum marginatum var. stenophyllum in Ganmao Qingre Granules |
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| DOI：10.16153/j.1002-7777.2023.04.013 |
| 中文关键词: 感冒清热颗粒 柴胡 藏柴胡 尼泊尔柴胡皂苷K 高效液相色谱-串联质谱 |
| 英文关键词: Ganmao Qingre granules Bupleuri Radix Bupleurum marginatum var. stenophyllum Nepasaikosaponin K HPLC-MS/MS |
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| 中文摘要: |
| 目的：建立感冒清热颗粒中藏柴胡的检查方法，考察柴胡的掺伪情况。方法：采用液相色谱串联质谱法，选择Agilent Poroshell 120 EC-C18(100 mm × 3.0 mm，2.7 μm)色谱柱，以乙腈-0.1% 甲酸溶液为流动相，梯度洗脱，流速 0.3 mL·min-1，柱温 35 ℃，进样量 5 μL；采用电喷雾离子源 (ESI)，选择m/z 943.5→797.5、m/z 943.5→781.2和m/z 943.5→635.5为尼泊尔柴胡皂苷K检测离子对，以多反应监测(MRM)模式进行测定。结果：尼泊尔柴胡皂苷K质量浓度在0.049~4.866 μg·mL-1范围内线性关系良好(r=0.9999)，精密度、重复性良好(RSD分别为1.42%、2.24%)。以0.8 μg·mL-1为掺伪判定浓度，220批感冒清热颗粒中有17批样品溶液尼泊尔柴胡皂苷K的浓度为1.2~3.5 μg·mL-1，判定为检出藏柴胡，不合格率7.7%。结论：建立的方法准确、可靠，可用于感冒清热颗粒中柴胡的掺伪检查及市场监管。 |
| 英文摘要: |
| Objective: To establish the inspection method of Bupleurum marginatum var. stenophyllum in Ganmao Qingre granules and investigate the adulteration of Bupleuri Radix. Methods: The high performance liquid chromatography-tandem mass spectrometry method was performed on Agilent Poroshell 120 EC-C18 (100 mm×3.0 mm, 2.7 μm) column, with mobile phase consisting of acetonitrile and 0.1% aqueous formic acid in gradient elution mode. The fl ow rate was 0.3 mL·min-1, the column temperature was set at 35 ℃ and the injection volume was 5 μL. The electrospray ionization source was used as detector, m/z 943.5→797.5, m/z 943.5→781.2 and m/z 943.5→635.5 were selected as the ion pairs and multiple reaction monitoring (MRM) mode was performed for the determination of Nepasaikosaponin K. Results: Nepasaikosaponin K showed good linear relationshipin the range of 0.049-4.866 μg·mL-1 (r=0.9999), the precision and repeatability were good, RSD were 1.42% and 2.24%, respectively, taking 0.8 μg·mL-1 as the determination concentration for adulteration, the concentration of Nepasaikosaponin K was between 1.2 and 3.5 μg·mL-1 of 17 samples in 220 batches of Ganmao Qingre granules, judged as the detection of Bupleurum marginatum var. stenophyllum, and the unqualifi ed rate was 7.7%. Conclusion: The established method is accurate and reliable, and can be applied to adulteration detection of Bupleuri Radix in Ganmao Qingre granules and market regulation. |
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