顶空毛细管气相色谱法同时测定罗库溴铵起始物料LK-7中的8种残留溶剂  

Determination of eight residual solvents in the starting material of rocuronium bromide by headspace capillary gas chromatography

作　　者：张丽姝 佘东来 王淼[1] 赵旻[1] 赵春杰[1] ZHANG Lishu;SHE Donglai;WANG Miao;ZHAO Min;ZHAO Chunjie(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Beijing Mega Pharmaceutical Science and Technology Co.,Ltd.,Beijing 100071,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]北京满格医药科技有限公司,北京100071

出　　处：《沈阳药科大学学报》2018年第7期547-551,共5页Journal of Shenyang Pharmaceutical University

摘　　要：目的采用顶空气相色谱法同时测定罗库溴铵起始物料LK-7中的8种残留溶剂。方法采用毛细管色谱柱Aglient DB-624(25 m×0.53 mm,3.0μm),程序升温,FID检测器,检测器温度:250℃,氮气为载气,流速:1.0 m L·min^(-1),采用顶空进样方式,进样口温度:200℃,顶空平衡温度:90℃,平衡时间:20 min。结果乙酸异丙烯酯、甲醇、二氯甲烷、三氯甲烷、吡啶、乙醚、2,4,6-三甲基吡啶、丙酮8种残留溶剂分别在0.030~0.301(r=1.000 0)、0.06~0.601(r=0.999 8)、0.013~0.126(r=0.999 8)、0.001~0.012(r=0.999 6)、0.004~0.041(r=0.999 8)、0.101~1.001(r=0.999 0)、0.004~0.042(r=1.000 0)、0.100~1.003 m L·min^(-1)(r=0.999 0)内线性关系良好,平均回收率分别为100.33%(RSD=1.04%)、93.68%(RSD=1.46%)、95.72%(RSD=1.67%)、91.03%(RSD=1.21%)、95.95%(RSD=1.34%)、91.77%(RSD=2.51%)、99.48%(RSD=0.89%)、95.42%(RSD=1.33%)。结论该方法可用于罗库溴铵起始物料中的残留溶剂检查。Objective To simultaneously determinate the eight residual solvents in the starting material of rocuronium bromide by headspace gas chromatography. Methods The separation was performed on a capillary column Aglient DB-624（ 25 m × 0. 53 mm,3. 0 μm） with a programmed temperature. The FID was used as a detector at 250 ℃,and nitrogen was used as the carrier with the flowrate of 1. 0 mL·min^-1. The headspace injection was utilized and the inlet temperature was 200 ℃. The equilibrium temperature was90 ℃ for 20 min. Results The calibration curves were linear within the range of 0. 030-0. 301（ r =1. 000 0）,0. 06-0. 601（ r = 0. 999 8）,0. 013-0. 126（ r = 0. 999 8）,0. 001-0. 012（ r = 0. 999 6）,0. 004-0. 041（ r = 0. 999 8）,0. 101-1. 001（ r = 0. 999 0）,0. 004-0. 042（ r = 1. 000 0）,and 0. 100-1. 003 mg·L^-1（ r = 0. 999 0） for isopropenyl acetater,methanol,dichloromethane,trichloromethane,pyridine,ether,2,4,6-trimethylpyridine and acetone. The average recoveries of eight components were 99. 49%（ RSD = 4. 07%）,95. 80%（ RSD = 3. 46%）,94. 93%（ RSD = 5. 89%）,85. 80%（ RSD =4. 90%）,96. 70%（ RSD = 3. 58%）,91. 03%（ RSD = 4. 00%）,99. 74%（ RSD = 6. 36%）,and 98. 17%（ RSD = 4. 10%）. Conclusion This method has high sensitivity and good accuracy,and can be used to detect residual solvents in the starting material of rocuronium bromide.

关 键 词：罗库溴铵起始物料 顶空气相色谱法 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]