顶空毛细管气相色谱法测定替卡西林钠原料药中的有机溶剂残留量  

Determination of Residual Organic Solvents in Ticarcillin Sodium by Headspace Capillary Gas Chromatography

作　　者：孙爱萍[1] 谷菲菲[1] 宋更申[2] 姜建国[2] 

机构地区：[1]河北化工医药职业技术学院机电工程系,石家庄市050026 [2]河北省药品检验所,石家庄市050011

出　　处：《中国药房》2011年第9期848-850,共3页China Pharmacy

摘　　要：目的:建立测定替卡西林钠原料药中甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯、甲苯6种有机溶剂残留量的方法。方法:采用顶空气相色谱法。色谱柱为DB-624石英毛细管柱,柱温采用程序升温,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为150℃,以水为溶解介质。结果:甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯、甲苯的检测浓度的线性范围分别为12.0～1200(r=0.9999)、10.0～1000(r=0.9998)、10.0～1000(r=0.9999)、1.20～120(r=0.9997)、10.0～1000(r=0.9998)、1.78～178μg·mL-1(r=0.9996);平均回收率为98.5%～99.6%(RSD=0.6%～2.0%);定量限为0.20～11.80μg·mL-1;3批样品中6种有机溶剂残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于该原料药中有机溶剂残留量的测定。OBJECTIVE： To establish the method for the content determination of 6 kinds of residual organic solvents in ticar- cillin sodium, i.e. methanol, alcohol, acetone, dichloromethane, ethyl acetate and methylbenzene. METHODS： Headspace GC was adopted. The residual organic solvents were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃. The inlet temperature was 150 ℃, and water was used as the solvent. RESULTS： The linear ranges of methanol, alcohol, acetone, dichloromethane, ethyl acetate and methylbenzene were 12.0~1 200 μg·mL^-1 （r=0.999 9）, 10.0~1 000 μg·mL^-1（r=0.999 8）, 10.0~1 000 μg·mL^-1 （r=0.999 9）, 1.20~120 μg·mL^-1 （r=0.999 7）, 10.0~1 000 μg·mL^-1（r=0.999 8）, 1.78~178 μg·mL^-1 （r=0.999 6）, respectively. The average recoveries were ranged from 98.5% to 99.6% with RSD of 0.6%~2.0%. The determination limits were 0.20--11.80 μg·mL^-1. The residual levels of 6 kinds of organic solvents in 3 batches of samples were all up to the standard stipulated in Chinese Pharmacopeia. CONCLUSION： The method is simple, accurate, sensitive and reproducible, and it can be used for the determination of residual organic solvents in ticarcil- lin sodium.

关 键 词：替卡西林钠 原料药 顶空毛细管气相色谱法 有机溶剂 残留量 

分 类 号：R927.2[医药卫生—药学] R978.11