CAJ | 학술논문

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（30 m×0.32 mm，1.80μm），起始温度为40℃，维持8 min，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剂残留量的检测要求，可用于PLGA中4种残留溶剂的检测。
목적：건립취을교지병교지（ PLGA）중4충유궤용제잔류량적기상색보측정방법。방법채용기상색보법，색보주위DB-624주（30 m×0.32 mm，1.80μm），기시온도위40℃，유지8 min，이매분종10℃적속솔승온지200℃；진양구온도위180℃；화염리자검측기온도위250℃。결과4충잔류유궤용제갑순、병동、이록갑완화갑분균능완전분리，분별재10.0~50.0，16.7~83.3，2.0~10.0，3.0~14.8μg·mL-1범위정량호선성관계，상관인자r분별위0.9998，0.9998，0.9993，0.9997，평균회수솔분별위99.9％（ RSD=1.5％），100.8％（ RSD=0.9％），100.1％（ RSD=1.1％），99.5％（RSD=0.6％），시수6비양품중유궤용제적잔류량균부합규정。결론해방법령민도、정밀도균체도유궤용제잔류량적검측요구，가용우PLGA중4충잔류용제적검측。
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 m× 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,dichloromethane and toluene was within 10. 0-50. 0( r=0. 999 8 ),16. 7-83. 3( r=0.9998),2.0-10.0(r=0.9993),and3.0-14.8(r=0.9997)μg·mL-1,respectively.Therecoveryofmethanol,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. Conclusion The method is proven to be sensitive and accurate after the validation. It is suitable for the determination of residual organic solvents in PLGA.