| 摘要: |
| 目的:建立院内制剂复方薄荷脑滴鼻液质量评价中含量测定的方法。 方法:采用气相色谱-质谱(GC-MS)测定薄荷脑和 樟脑含量。 GC-MS 条件:色谱柱 Agilent DB-5MS(30 m×250 μm×0. 25 μm),流速 1 mL/ min,分流比 10 ∶ 1,进样口温度 300 ℃ ,程 序升温(90 ℃保持 5 min,以 1 ℃ / min 升至 100 ℃ ,保持 5 min,以 10 ℃ / min 升至 220 ℃ ,保持 2 min);质谱离子源:电子轰击 (EI)源,温度 230 ℃,四级杆温度 150 ℃,电子能量 70 eV,质荷比(m/ z)30~800。 结果:薄荷脑和樟脑分别在 50. 20~803. 20 μg / mL (r = 0. 999 6)和 50. 10~801. 60 μg / mL(r = 0. 999 4)浓度范围内与峰面积呈现良好的线性关系,平均回收率 101. 5%和 101. 1%,精 密度、稳定性、重复性实验结果相对标准偏差(RSD)均<2%。 结论:初步建立了复方薄荷脑滴鼻液中薄荷脑和樟脑的含量测定 方法,通过 GC-MS 建立的质量标准准确、重复性好,可用于复方薄荷脑滴鼻液中薄荷脑和樟脑的含量测定和质量控制。 |
| 关键词: 复方薄荷脑滴鼻液 薄荷脑 樟脑 气相色谱-质谱 |
| DOI：10.13407/j.cnki.jpp.1672-108X.2023.11.010 |
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| 基金项目:天津市教委科研计划项目,编号 2020KJ203 |
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| Simultaneous Content Determination of Menthol and Camphor in Compound Menthol Nasal Drops by Gas Chromatography-Mass Spectrometry |
| Yang Liu1 , Zhou Yaxuan1 , Zhang Nan1 , Wang Xue2 |
| (1. Tianjin Children’ s Hospital, Tianjin 300134, China; 2. Tianjin Medical University, Tianjin 300070, China) |
| Abstract: |
| Objective: To establish the method for content determination in quality evaluation of compound menthol nasal drops. Methods: Gas chromatography-mass spectrometry ( GC-MS ) was adopted to determine levels of menthol and camphor. GC-MS conditions included Agilent DB-5MS column ( 30 m × 250 μm × 0. 25 μm), flow rate of 1 mL/ min, split ratio of 10 ∶ 1, injector temperature of 300 ℃ , and temperature program (initial temperature of 90 ℃ for 5 min, followed by increase of 1 ℃ / min to 100 ℃ with 5-minute hold, and increase of 10 ℃ / min to 220 ℃ with 2-minute hold). The mass spectrometer used an electron impact (EI) source with temperature of 230 ℃ , quadrupole temperature of 150 ℃ , electron energy of 70 eV, and mass-to-charge ratio (m/ z) range of 30 to 800. Results: Menthol and camphor exhibited excellent linear relationships with peak areas within concentration ranges of 50. 20 to 803. 20 μg / mL (r = 0. 999,6) and 50. 10 to 801. 60 μg / mL (r = 0. 999,4), respectively. The average recovery rates were 101. 5% and 101. 1% for menthol and camphor, respectively. The precision, stability and repeatability experiments yielded relative standard deviations (RSD) of less than 2%. Conclusion: A preliminary quantitative analysis method for menthol and camphor in compound menthol nasal drops has been established. The quality standards developed by using GC-MS are accurate and exhibit good reproducibility, which can be applied for the content determination and quality control of menthol and camphor in compound menthol nasal drops. |
| Key words: compound menthol nasal drops menthol camphor gas chromatography-mass spectrometry |
