HPLC-ELSD法检测4-(4'-正丙基环己基)-环己基甲醛顺反异构体
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摘要
目的:建立了一种测定4-(4'-正丙基环己基)-环己基甲醛顺反异构体的反相HPLC-ELSD法。方法:采用Inter Sustain Swift C18(150×4.6 mm,5μm)色谱柱,以乙醇∶水(V/V=80∶20)为流动相,流速为1.0 mL/min,漂移管温度为35℃,雾化气压力350 kPa。结果:在选定的色谱条件下,4-(4'-正丙基环己基)-环己基甲醛顺式异构体和反式异构体可达到很好的分离,在0.1～0.5μg/mL线性范围内顺反异构的相对矫正因子为0.95,顺式异构体的平均回收率为100.3%,最低检出量为200 ng。结论:方法快速简便,重现性好,可用于控制反式4-(4'-正丙基环己基)-环己基甲醛中的顺式异构体。
Objective:A method for determination of trans and cis isomers of 4-(4'-propylcyclohexyl)-cyclohexyl formaldehydein was established. Method: The method adopted an evaporative light-scattering detector(ELSD). The separation was carried out on a Inter Sustain Swift C18(150×4.6 mm, 5 μm). The mobile phase consisted of ethanol-water(80∶20)at a flowrate of 1.0 mL/min, the temperature of the drift tube was set at 35℃,and the nebulizer pressure at 350 kPa.Results: Good separation of trans and cis could be achieved under the above system, the relative correction factor of cis was0.95 range from 0.1 μg/m to 0.5 μg/m. The limits of detection was 200 ng and the recoveries was 100.3%. Conclusion: An excellent method to control cis impurity in trans sample was proposed with fast, simple and good reproducible characters.
Objective:A method for determination of trans and cis isomers of 4-(4'-propylcyclohexyl)-cyclohexyl formaldehydein was established. Method: The method adopted an evaporative light-scattering detector(ELSD). The separation was carried out on a Inter Sustain Swift C18(150×4.6 mm, 5 μm). The mobile phase consisted of ethanol-water(80∶20)at a flowrate of 1.0 mL/min, the temperature of the drift tube was set at 35℃,and the nebulizer pressure at 350 kPa.Results: Good separation of trans and cis could be achieved under the above system, the relative correction factor of cis was0.95 range from 0.1 μg/m to 0.5 μg/m. The limits of detection was 200 ng and the recoveries was 100.3%. Conclusion: An excellent method to control cis impurity in trans sample was proposed with fast, simple and good reproducible characters.
引文
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[2]白木,子萌.新一代OLED显示技术[J].现代显示,2002(3):14-17.
[3]王明娟,胡昌勤,金少鸿,等.采用HPLC-ELSD法分析小诺霉素及其有关物质[J].药物分析杂志,2002(3):205-208.
[4]徐兴亚,李倚云. HPLC-ELSD法同时测定新氢化可的松乳膏中硫酸新霉素和氢化可的松的含量[J].实用药物与临床,2011,14(2):140-142.