气相色谱法测定注射用血栓通(冻干)中两种成分的残留  

Determination of Residual Amounts of Two Compounds in Xueshuantong for Injection(Lyophilized)by Gas Chromatography

作　　者：覃济桓 张兆佳 王海燕 刘冠萍 梁云飞 

机构地区：[1]广西中恒创新医药研究有限公司,广西南宁530031 [2]广西三七综合利用技术重点实验室,广西梧州543000

出　　处：《大众科技》2020年第8期45-47,79,共4页Popular Science & Technology

摘　　要：目的:建立GC方法,考察药用氯化丁基橡胶塞中甲基环戊烷和环己烷在药品中的迁移情况。方法:采用DB-5色谱柱(30 m×0.53 mm,2.65μm);进样口:200℃;FID检测器温度:250℃;柱温程序:起始温度40℃,保持5 min,以4℃·min^-1速率升至100℃,再以6℃·min^-1速率升温至160℃,再以20℃·min^-1速率升温至240℃,保持2分钟;载气:氮气,流速3.2 mL·min^-1;顶空条件:Oven:121℃保持30 min,Loop:150℃,Line:160℃。结果:甲基环戊烷和环己烷分别在浓度3.68μg·mL-1~735.6μg·mL^-1和4.21μg·mL^-1~841.5μg·mL^-1范围内线性良好(r≥0.9993);甲基环戊烷和环己烷在橡胶塞中的提取重复性范围分别是0.3847μg·g^-1~0.4357μg·g^-1(n=6,RSD=4.6%)和0.3003μg·mL^-1~0.3345μg·mL^-1(n=6,RSD=4.04%);甲基环戊烷和环己烷提取回收率范围分别是98%~110%(n=9,RSD=4.59%)及86%~97%(n=9,RSD=4.82%)。结论:本方法灵敏、准确、可靠,可用于药用氯化丁基橡胶塞中甲基环戊烷和环己烷的提取和迁移研究。Objective:To establish the GC method for investigating the migration of methylcyclopentane and cyclohexane in medicinal chlorinated butyl rubber plugs.Methods:The DB-5 column(30 m×0.53 mm,2.65μm);Inlet:200℃;FID detector temperature:250℃;column temperature program:starting temperature 40℃,hold 5 min,rise to 100℃at 4℃·min^-1,then increase the temperature to 160℃at 6℃·min^-1,and then increase the temperature to 240℃at 20℃·min-1 for 2 minutes;carrier gas:nitrogen,flow rate 3.2 mL·min^-1;headspace conditions:Oven:121℃to maintain 30 min,Loop:150℃,Line:160℃.Results:Methylcyclopentane and cyclohexane were linear at concentrations of 3.68μg·g^-1 to 735.6μg·mL^-1 and 4.21μg·g^-1 to 841.5μg·mL^-1,respectively(r≥0.9993);extraction repeatability range of methylcyclopentane and cyclohexane in rubber stopper was 0.3847μg·g^-1 to 0.4357μg·g^-1(n=6,RSD=4.6%)and 0.3003μg·mL^-1 to 0.3345μg·mL^-1(n=6,RSD=4.04%);the extraction recovery range of methylcyclopentane and cyclohexane was 98%to 110%(n=9,RSD=4.59%)and 86%to 97%(n=9,RSD=4.82%).Conclusion:The method is sensitive,accurate and reliable,and can be used for the extraction and migration of methylcyclopentane and cyclohexane in the medicinal chlorinated butyl rubber plugs.

关 键 词：气相色谱 甲基环戊烷 环己烷 注射用血栓通(冻干) 

分 类 号：R927.1[医药卫生—药学]