【摘要】：目的:建立氣相色譜法,同時(shí)測(cè)定藥用輔料中二氯甲烷、三氯甲烷、三氯乙烯、1,4-二氧雜環(huán)己烷4種揮發(fā)性有機(jī)雜質(zhì)。方法:使用DB-WAX(30.0 m×250μm×0.25μm)彈性毛細(xì)管柱,進(jìn)樣口溫度200℃,分流比10∶1,恒流流速1.0 m L·min-1,檢測(cè)口溫度230℃,柱溫為程序升溫(起始溫度35℃,保持5 min,8℃·min-1升至70℃,以50℃·min-1升至180℃),頂空平衡溫度140℃,時(shí)間30 min。結(jié)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%,1,4-二氧雜環(huán)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%,1,4-二氧雜環(huán)己烷1.55%。3種輔料中有機(jī)揮發(fā)性雜質(zhì)檢測(cè)結(jié)果:交聯(lián)羧甲基纖維素鈉中三氯甲烷質(zhì)量分?jǐn)?shù)為0.67~1.88μg·g-1,二氯甲烷、三氯乙烯及1,4-二氧雜環(huán)己烷未檢出;微粉硅膠中二氯甲烷質(zhì)量分?jǐn)?shù)為1.12~3.25μg·g-1、三氯甲烷、三氯乙烯及1,4-二氧雜環(huán)己烷未檢出;微晶纖維素中二氯甲烷質(zhì)量分?jǐn)?shù)為0.91~1.39μg·g-1,三氯甲烷質(zhì)量分?jǐn)?shù)為1.03~2.36μg·g-1,三氯乙烯質(zhì)量分?jǐn)?shù)為0.09~0.28μg·g-1,1,4-二氧雜環(huán)己烷未檢出。結(jié)論:本法經(jīng)方法學(xué)驗(yàn)證,適用于交聯(lián)羧甲基纖維素鈉、微粉硅膠及微晶纖維素中有機(jī)揮發(fā)性雜質(zhì)的檢測(cè)。
[Abstract]:Objective: to establish a gas chromatographic method for the simultaneous determination of four volatile organic impurities including dichloromethane, trichloroethylene and 1-dioxa-cyclohexane in medicinal excipients. Methods: the DB-WAX (30.0 m 脳 250 渭 m 脳 0.25 渭 m) elastic capillary column was used. The injection temperature was 200 鈩，

本文編號(hào)：2358905