顶空-气相色谱法检测卤化丁基胶塞中的挥发性化合物  

Determination of Volatile Compounds in Halogenated Butyl Rubber Stoppers by Headspace-Gas Chromatography

作　　者：班璐 于兰[1] 马玉玲 白青青 张晴[1] 王娅莉 BAN Lu;YU Lan;MA Yuling;BAI Qingqing;ZHANG Qing;WANG Yali(National Engineering Research Center of Microbial Medicine,Hebei Industry Microbial Metabolic Technology Innovation Center,Shijiazhuang Microbial Medicine Technology Innovation Center,New Drug Research&Development Company of NCPC,Shijiazhuang 052165,China)

机构地区：[1]微生物药物国家工程研究中心、河北省工业微生物代谢技术创新中心、石家庄市微生物药物技术创新中心、华北制药集团新药研究开发有限责任公司,河北石家庄052165

出　　处：《化学与生物工程》2023年第10期64-68,共5页Chemistry & Bioengineering

基　　金：河北省科技研发平台建设专项(22567651H)。

摘　　要：建立了顶空-气相色谱法检测注射用阿尼芬净的卤化丁基胶塞中的2-甲基戊烷、3-甲基戊烷、正己烷、甲基环戊烷、环己烷等5种挥发性化合物。采用DB-624色谱柱,起始温度60℃保持3 min,以5℃•min^(-1)升温到80℃保持10 min,再以15℃•min^(-1)升温到240℃保持10 min,分流比20∶1,顶空瓶80℃平衡40 min。在上述条件下,5种挥发性化合物的分离度均大于1.5,其浓度均在0.1-20μg•mL^(-1)范围内与峰面积线性关系良好,加标回收率均在81.1%-101.7%之间,相对标准偏差均小于10%。该方法专属性强、重现性好、准确度高,可用于包装材料与药品相容性试验中的可挥发性化合物的检测。A headspace-gas chromatography is developed for the determination of five volatile compounds(namely,2-methylpentane,3-methylpentane,hexane,methyl cyclopentane,and cyclohexane)in halogenated butyl rubber stoppers of Anidulafungin for injection.The separation degree of five compounds is greater than 1.5 under the conditions as follows:DB-624 column is adopted with the initial temperature of 60℃for 3 min,raising the temperature to 80℃at 5℃•min^(-1) for 10 min,and raising the temperature to 240℃at 15℃•min^(-1) for 10 min,the split ratio is 20∶1 and the sample is equilibrated at 80℃ for 40 min.Five volatile compounds have a good linear relationship with peak area in the range of 0.1-20μg•mL^(-1).The recoveries are 81.1%^(-1)01.7%with the relative standard deviations less than 10%.The determination method has strong specificity,good reproducibility,and high accuracy,which can be used to detect volatile compounds in the compatibility test of packaging materials and drugs.

关 键 词：顶空-气相色谱法 卤化丁基胶塞 挥发性化合物 包装材料 相容性 

分 类 号：O657.7[理学—分析化学] R927.1[理学—化学]