聚乙交酯丙交酯中有机溶剂残留的测定  

Determination of Residual Organic Solvents in Poly(lactic-co-glycolide)

作　　者：帅放文 章家伟 王向峰 张婷 王宇彤[4] 周宏灏[3] 

机构地区：[1]湖南省药用辅料工程技术研究中心,长沙410331 [2]湖南尔康制药股份有限公司,长沙410331 [3]中南大学临床药理研究所,长沙410078 [4]中国药科大学药剂教研室,南京210009

出　　处：《医药导报》2014年第6期775-778,共4页Herald of Medicine

基　　金：科技部重大新药创制项目(2013ZX09509106)

摘　　要：目的建立聚乙交酯丙交酯（PLGA）中4种有机溶剂残留量的气相色谱测定方法。方法采用气相色谱法，色谱柱为DB-624柱（30m×0．32mm，1．80μm），起始温度为40℃，维持8min，以每分钟10℃的速率升温至200℃；进样口温度为180℃；火焰离子检测器温度为250℃。结果4种残留有机溶剂甲醇、丙酮、二氯甲烷和甲苯均能完全分离，分别在10．0～50．0，16．7～83．3，2．0～10．0，3．0—14．8μg·mL^-1范围呈良好线性关系，相关因子r分别为0．9998，0．9998，0．9993，0．9997，平均回收率分别为99．9％（RSD=1．5％），100．8％（RSD=0．9％），100．1％（RSD=1．1％），99．5％（RSD=0．6％），市售6批样品中有机溶剂的残留量均符合规定。结论该方法灵敏度、精密度均达到有机溶刑残留量的检测要求，可用于PLGA中4种残留溶剂的检测。Objective To establish a capillary gas chromatography （GC） method for the determination of residual organic solvents in poly （lactic-co-glycolide） （ PLGA ） , including methanol, acetone, dichloromethane, and toluene. Methods A capillary GC method was carried out. DB-624 capillary column （30 mm× 0.32 mm, 1.80 μm） with programmed temperature chromatography was employed. The initial temperature was kept at 40 ℃ for 8 min. Then the temperature was raised to 200 ℃ at a rate of 10 ℃ · min-1. The injection port temperature was 180 ℃ ,and the split ratio was 10 ： 1. The carrier gas was nitrogen. The temperature of FID was set at 250 ℃, and the sample volume was set at 3 μL. Results Four residual organic solvents consisting of methanol, acetone, dichloromethane and toluene in PLGA were completely separated. The linear range of concentration of methanol, acetone, diehloromethane and toluene was within 10.0 - 50.0 （ r = 0. 999 8 ） , 16.7 - 83.3 （ r = 0. 999 8） ,2.0-10.0 （r=0.999 3） ,and 3.0-14.8 （r=0. 999 7） μg · mL^-1 ,respectively. The recovery of methanol,acetone, dichloromethane and toluene was 99.9% （ RSD = 1.5% ）, 100.8% （ RSD = 0.9% ）, 100. 1% （ RSD = 1. 1% ） , and 99.5% （ RSD = 0.6% ） , respectively. Six batches of samples met the requirements. Condusion The method is proven to be sensitive and accurate after the validation. It is suitable for the determination of residual organic solvents in PLGA.

关 键 词：聚乙交酯丙交酯 色谱法 气相 残留溶剂 

分 类 号：R927.2[医药卫生—药学]