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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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异氟烷有关物质和残留溶剂的测定

Determination of related substances and residual solvents in isoflurane

作者(英文):
分类号:R917
出版年·卷·期(页码):2018,38 (12):2116-2121
DOI: 10.16155/j.0254-1793.2017.01.01
-----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,0.25 μm);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、0.002~0.02 μL·mL-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 4 μg·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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------
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