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目的:建立气相色谱法,同时测定药用辅料中二氯甲烷、三氯甲烷、三氯乙烯、1,4-二氧杂环己烷4种挥发性有机杂质。方法:使用DB-WAX(30.0 m×250μm×0.25μm)弹性毛细管柱,进样口温度200℃,分流比10∶1,恒流流速1.0 m L·min-1,检测口温度230℃,柱温为程序升温(起始温度35℃,保持5 min,8℃·min-1升至70℃,以50℃·min-1升至180℃),顶空平衡温度140℃,时间30 min。结果:回收率:二氯甲烷100.3%~100.6%,三氯甲烷101.3%~101.8%,三氯乙烯100.9%~101.4%,1,4-二氧杂环己烷99.6%~100.1%;精密度的RSD:二氯甲烷1.65%,三氯甲烷2.25%,三氯乙烯2.00%,1,4-二氧杂环己烷1.55%。3种辅料中有机挥发性杂质检测结果:交联羧甲基纤维素钠中三氯甲烷质量分数为0.67~1.88μg·g-1,二氯甲烷、三氯乙烯及1,4-二氧杂环己烷未检出;微粉硅胶中二氯甲烷质量分数为1.12~3.25μg·g-1、三氯甲烷、三氯乙烯及1,4-二氧杂环己烷未检出;微晶纤维素中二氯甲烷质量分数为0.91~1.39μg·g-1,三氯甲烷质量分数为1.03~2.36μg·g-1,三氯乙烯质量分数为0.09~0.28μg·g-1,1,4-二氧杂环己烷未检出。结论:本法经方法学验证,适用于交联羧甲基纤维素钠、微粉硅胶及微晶纤维素中有机挥发性杂质的检测。
OBJECTIVE: To establish a gas chromatographic method for the simultaneous determination of four volatile organic compounds, dichloromethane, trichloromethane, trichlorethylene and 1,4-dioxane in pharmaceutical excipients. Methods: A capillary column with DB-WAX (30.0 m × 250 μm × 0.25 μm) was used. The inlet temperature was 200 ℃, the split ratio was 10:1, the flow rate was 1.0 m L · min-1, Temperature was programmed temperature (initial temperature 35 ℃, hold 5 min, 8 ℃ · min-1 rose to 70 ℃, 50 ℃ · min-1 rose to 180 ℃), the equilibrium temperature was 140 ℃ for 30 min. Results: The recoveries were 100.3% ~ 100.6% for dichloromethane, 101.3% ~ 101.8% for trichloromethane, 100.9% ~ 101.4% for trichlorethylene and 99.6% ~ 100.1% for 1,4-dioxane. RSD: 1.65% dichloromethane, 2.25% chloroform, 2.00% trichlorethylene and 1.55% 1,4-dioxane. Three kinds of excipients organic volatile impurities test results: Croscarmellose sodium in chloroform mass fraction of 0.67 ~ 1.88μg · g-1, dichloromethane, trichlorethylene and 1,4-dioxa Cyclohexane was not detected. The mass fraction of methylene chloride in the silica gel was 1.12-3.25μg · g-1, while the chloroform, trichlorethylene and 1,4-dioxane were not detected. The microcrystalline fibers The content of methylene dichloride was 0.91 ~ 1.39μg · g-1, the mass fraction of trichloromethane was 1.03 ~ 2.36μg · g-1, the mass fraction of trichlorethylene was 0.09 ~ 0.28μg · g-1,1,4 - Dioxane was not detected. Conclusion: This method is validated by methodology and is suitable for the detection of organic volatile impurities in croscarmellose sodium, powdered silica gel and microcrystalline cellulose.