摘要
目的:完善和建立异氟烷有关物质和残留溶剂的测定方法。方法:采用2-硝基对苯二酸改性的聚乙二醇(FFAP)(或极性相似)为固定液的毛细管柱(30 m×0.32 mm,0.25μm);氢火焰离子化检测器;载气为氮气,流速为1 mL·min^(-1),分流比为10∶1,程序升温(起始温度为55℃,维持7 min;以30℃min^(-1)的速率升温至210℃,维持15 min;以10℃min^(-1)的速率升温至240℃,维持3 min);进样口温度为150℃;检测器温度为250℃。结果:1-氯-2,2,2-三氟乙基氯二氟甲基醚(异氟烷杂质A)、2,2,2-三氟乙基二氟甲基醚(异氟烷杂质B)、丙酮、N,N-二甲基甲酰胺分别在0.02～0.2、0.0 144～0.144、0.02～0.2、0.002～0.02μL·m L^(-1)范围内呈良好的线性关系,平均回收率分别为101.7%、101.6%、99.0%、97.6%,RSD分别为3.0%、2.5%、2.1%、2.3%,检测下限分别为0.003、0.006 48、1.099 9、0.758 4μg·mL^(-1)。结论:建立的方法可用于异氟烷有关物质和残留溶剂的测定,能更有效地控制异氟烷的质量。
Objective:To establish a method for the determination of related substances and residual solvents in isoflurane.Methods:The residual organic solvents were determined by GC with capillary column(FFAP),FID detector and nitrogen as carrier gas.The temperature of the injection port was 150 ℃ and the detector temperature was 250℃.The initial column temperature was 55℃,maintaining 7 min,and the temperature was raised to 210℃ at a rate of 30 ℃·min^-1,maintaining 15 min.The temperature was raised to 240 ℃ at a rate of 10 ℃·min-1, maintaining 3 min.The flow rate of N2 was 1.0 mL·min^-1.Results:The calibration curve showed a good linearity with the range of 0.02-0.2 μL·mL^-1 for isoflurane related compound A(r2=0.994),with the range of 0.0 144- 0.144 μL·mL^-1 for isoflurane related compound B(r2=0.995),with the range of 0.02-0.2 μL·mL^-1 for acetone (r2=0.993)and with the range of 0.002-0.02 μL·mL^-1 for N,N-dimethyl formamide(r2=0.992).The average recoveries(n=9)of isoflurane related compound A,isoflurane related compound B,acetone and N,N-dimethyl formamide were 101.7%(RSD=3.0%),101.6%(RSD=2.5%),99.0%(RSD=2.1%)and 97.6%(RSD= 2.3%).The detection limits of isoflurane related compound A,isoflurane related compound B,acetone and N, N-dimethyl formamide were 0.003 μg·mL^-1,0.006 48 μg·mL^-1,1.099 9 μg·mL^-1 and 0.758 4 μg·mL^-1. Conclusion:This method is accurate,reliable and sensitive for the determination of related substances and residual solvents in isoflurane.
作者
马玲
陈欢
黄钰馨
沈晓华
刘瑞
撖志明
刘加
MA Ling;CHEN Huan;HUANG Yu-xin;SHEN Xiao-hua;LIU Rui;HAN Zhi-ming;LIU Jia(Ningxia Institute of Drug Control,Yinchuan 750001,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第12期2116-2121,共6页
Chinese Journal of Pharmaceutical Analysis
关键词
异氟烷
有关物质
残留溶剂
毛细管气相色谱法
标准提高.
isoflurane
related substances
residual solvents
capillary gas chromatography
standardimprovement
