摘要
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 set up a method of capillary GC to determine dichloromethane, chloroform, trichloroethylene and 1,4-dioxane in conventional officinal accessories. Methods： A DB-WAX （30.0 m × 250 μm × 0.25 μm）elastic capillary column was adopted. The inlet temperature was 200℃ , the split ratio was 10：1 , the constant flow was 1.0 mL ·min-1 , and the detection temperature was 230℃. The column temperature programming was used （initial temperature was 35 ℃ , held for 5 rain, raised to 70 ℃ at a rate of 8 ℃· min-1 ,then raised to 180 ℃ at a rate of 50 ℃ · min-1）. The headspace balance temperature was 140 ℃ , and the balance time was 30 min. Results ： The recovery rates of dichloromethane, chloroform, trichloroethylene andl,4-dioxanewere 100.3%-100.6%,101.3%-101.8%,100.9%-101.4% and99.6% - 100.1% , respectively. The RSDs of precision of dichloromethane, chloroform, trichloroethylene and 1 , 4 -dioxane were 1.65% ,2.25% ,2.00% and 1.55% , respectively. The testing results of organic volatile impurities in 3 kinds of accessories were as follows. The mass fraction of chloroform in croscarmellose sodium was 0.67- 1.88 μg· g-1 ; dichloromethane, trichloroethylene and 1,4-dioxane were undetected. The content of dichloromethane in silicon dioxide was 1. 12 - 3.25 μg·g- 1 ; chloroform, trichloroethylene and 1,4- dioxane were undetected. The contents of dichloromethane, chloroform and trichloroethylene in micro- crystalline cellulose were 0.91 - 1 . 39 μg · g-1 , 1 . 03 -2.36 μg · mL-1 and 0.09 - 0.28 μg· g-1 ;1,4- dioxane was undetected. Conclusion ： Through the verification of methodology, this method is applicable to the detection of organic volatile impurities in croscarmellose sodium, silicon dioxide and microcrystalline cellulose.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第11期2012-2017,共6页
Chinese Journal of Pharmaceutical Analysis
基金
中医药行业科研专项项目(200807032)
