摘要: |
目的:建立测定清宣止咳颗粒中薄荷脑含量的气相色谱法。方法:采用DB-FFAP 弹性石英毛细管柱(25 m×0. 32 mm×
0. 50 μm);FID 检测器;载气: N2;流速1 mL/ min,进样口温度200 ℃,检测器温度250 ℃;柱温: 初始温度70 ℃,保持4 min,然后以
10 ℃ / min 升温至120 ℃,保持5 min,再以5 ℃ / min 升温至180 ℃,保持2 min,最后以25 ℃ / min 升温至200 ℃,保持5 min;进样量
1 μL;分流比2 ∶ 1。结果:薄荷脑质量浓度在0. 01~0. 10 mg/ mL 范围内与峰面积呈良好线性关系(r = 0. 998 5),平均回收率为
99. 9%(n =9,RSD=3. 8%)。结论:本方法快速、简便,结果可靠、准确,重现性好,适用于清宣止咳颗粒中薄荷脑含量的测定。 |
关键词: 气相色谱法 清宣止咳颗粒 薄荷脑 含量 |
DOI:doi:10.13407/j.cnki.jpp.1672-108X.2024.04.001 |
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基金项目: |
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Content Determination of Menthol in Qingxuan Zhike Granules by Gas Chromatography |
Kong Fanjian1, Su Qishuang2 |
((1. Yuxi Food and Drug Inspection Institute, Yunnan Yuxi 653100, China; 2. Yunnan University of
Chinese Medicine, Kunming 650500, China)) |
Abstract: |
Objective: To establish the gas chromatography method for content determination of Qingxuan Zhike granules. Methods:
Gas chromatography was used with DB-FFAP elastic quartz capillary column (25 m×0. 32 mm×0. 50 μm). FID detector; carrier gas:
N2 were used, with flow rate of 1 mL/ min, inlet temperature of 200 ℃, detector temperature of 250 ℃. The initial temperature was 70 ℃,
maintained for 4 min, then increased to 120 ℃ at a rate of 10 ℃ / min, maintained for 5 min, and then increased to 180 ℃ at a rate of
5 ℃ / min, maintained for 2 min, the temperature increased to 200 ℃ at the rate of 25 ℃ / min and maintained for 5 min. The injection
volume was 1 μL, with split ratio of 2 ∶ 1. Results: Menthol showed a good linear relationship in the range of 0. 01 to 0. 10 mg/ mL
(r =0. 998,5), and the average recovery was 99. 9% (n = 9, RSD = 3. 8%). Conclusion: The method is rapid, simple, reliable,
accurate and reproducible, which is suitable for the determination of menthol in Qingxuan Zhike granules. |
Key words: gas chromatography Qingxuan Zhike granules menthol content |