| 吴凤如.气相色谱法测定氟米龙残留溶剂的方法研究[J].中国药品标准,2018,19(3):196-199 |
| 气相色谱法测定氟米龙残留溶剂的方法研究 |
| Determination of Residual Solvents in Fluorometholone by GCWu Fengru (Guangdong Institute For Drug Control, Guangzhou, Guangdong 510180, China) |
| 投稿时间：2017-12-08 修订日期：2018-06-11 |
| DOI： |
| 中文关键词: 氟米龙 残留溶剂 气相色谱 |
| 英文关键词: fluorometholone residual solvents GC method |
| 基金项目: |
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| 中文摘要: |
| 目的：建立气相色谱法测定氟米龙中甲醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃与吡啶残留量的方法。方法：采用以6％氰丙基苯基-94％二甲基硅氧烷(或极性相近)为固定液的毛细管柱，FID检测器，以氮气为载气，二甲基亚砜为溶剂，顶空进样。结果：在选定的色谱条件下，各成分可达到很好的分离；甲醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃与吡啶分别在0.6～150，0.1～75，0.6～20，0.3～8，0.2～7.5，4～15μ g·mL-1 的范围内线性良好（r=0.9950~0.9999）；精密度、重复性的RSD均不大于5.0%；回收率分别为100.7%、98.2%、95.8%、94.5%、94.7%、97.5%（n=9，RSD＜3%）。甲醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃、吡啶的定量限分别为2μ g·mL-1、0.5μ g·mL-1、1μ g·mL-1、1μ g·mL-1、1μ g·mL-1、10μ g·mL-1；检测限分别为0.6μ g·mL-1、0.1μ g·mL-1、0.6μ g·mL-1、0.3μ g·mL-1、0.2μ g·mL-1、4μ g·mL-1。测定供试品3批，供试品一甲醇检出量为0.01%，丙酮检出量为0.003%，二氯甲烷、乙酸乙酯、四氢呋喃、吡啶均未检出；供试品二甲醇检出量为0.02%，丙酮检出量为0.006%，二氯甲烷、乙酸乙酯、四氢呋喃、吡啶均未检出；供试品三甲醇检出量为0.02%，丙酮检出量为0.006%，二氯甲烷、乙酸乙酯、四氢呋喃、吡啶均未检出。 |
| 英文摘要: |
| Objective: To establish a GC method for determining residual solvents —— methanol, acetone, dichloromethane, ethyl acetate, tetrahydrofuran and pyridine in raw meterial drug of Fluorometholone. Methods: The GC method with head-space sampling was equipped with FID as detector and DMSO as the solvent. A capillary column with 6% cyano phenyl -94% two methyl siloxane (or similar polarity) as stationary solution (30m×0.53nm×3.0μm). The carrier gas was nitrogen. Results: Each component can be separated well. There were good linear relationship with r=0.995 0-0.999 9 in the range of 0.6-150μ g·mL-1，0.1-75μ g·mL-1，0.6-20μ g·mL-1，0.3-8μ g·mL-1，0.2-7.5μ g·mL-1，4-15μ g·mL-1 for methanol, acetone, dichloromethane, ethyl acetate, tetrahydrofuran and pyridine. The RSDs of the precision、 repeatability were not more than 5.0%. The recoveries were 100.7%、98.2%、95.8%、94.5%、94.7% and 97.5% for methanol, acetone, dichloromethane, ethyl acetate, tetrahydrofuran and pyridine.（ n=9，RSD＜3%）. The limits of quantitation of methanol, acetone, dichloromethane, ethyl acetate, tetrahydrofuran and pyridine were 2μ g·mL-1,0.5μ g·mL-1,1μ g·mL-1,1μ g·mL-1,1μ g·mL-1,10μ g·mL-1 .The limits of detection of methanol, acetone, dichloromethane, ethyl acetate, tetrahydrofuran and pyridine were 0.6μ g·mL-1 ,0.1μ g·mL-1,0.6μ g·mL-1,0.3μ g·mL-1,0.2μ g·mL-1,4μ g·mL-1 .Third batches of samples were tested. 0.01% methanol and 0.003% acetone were detected, and dichloromethane, ethyl acetate, tetrahydrofuran , pyridine were not detected in sample 1. 0.02% methanol and 0.006% acetone were detected, and dichloromethane, ethyl acetate, tetrahydrofuran ,pyridine were not detected in sample2. 0.02% methanol and 0.006% acetone were detected, and dichloromethane, ethyl acetate, tetrahydrofuran , pyridine were not detected in sample3. Conclusion: The method is sensitive, accurate, specific and suitable for the determination of residual solvents in fluorometholone. |
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