CAJ | 학술논문

目的：建立硝酸咪康唑原料残留溶剂的测定方法。方法采用气相色谱法，使用 PEG-20M 毛细管（30 m ×0．25 mm ，0．25μm ）色谱柱，柱温采用程序升温，初始温度60℃，保持3 min ，再以30℃· min-1升至185℃，保持20 min；进样口温度为200℃；检测器为FID ；检测器温度为250℃。结果同时测定了硝酸咪康唑原料中的2种有机溶剂，丙酮和甲苯线性范围分别为0．25～1．0mg·mL -1（r＝0．9998）、0．0445～0．178mg·mL -1（r＝0．9996），平均加样回收率分别为100．3％和99．9％， RSD分别为1．8％和1．3％。结论该方法灵敏、准确，可用于硝酸咪康唑中残留溶剂的检测。
목적：건립초산미강서원료잔류용제적측정방법。방법채용기상색보법，사용 PEG-20M 모세관（30 m ×0．25 mm ，0．25μm ）색보주，주온채용정서승온，초시온도60℃，보지3 min ，재이30℃· min-1승지185℃，보지20 min；진양구온도위200℃；검측기위FID ；검측기온도위250℃。결과동시측정료초산미강서원료중적2충유궤용제，병동화갑분선성범위분별위0．25～1．0mg·mL -1（r＝0．9998）、0．0445～0．178mg·mL -1（r＝0．9996），평균가양회수솔분별위100．3％화99．9％， RSD분별위1．8％화1．3％。결론해방법령민、준학，가용우초산미강서중잔류용제적검측。
Objective To establish a method for the determination of two residual solvents in miconazole nitrate .Methods The de-termination was performed on a GB-WAX column (30 m × 0 .25 mm ,0 .25 μm) .The column temperature was maintained at 60 ℃for 3 min ,and programmed to 185 ℃ at 30 ℃ · min-1 ,then held for 20 min .FID was used as a detector ,and the temperatures of the injector and detector were set at 200 and 250 ℃ ,respectively .Results Two organic solvents of miconazole nitrate were deter-mined simultaneously in raw materials .The calibration curves were linear in the ranges of 0 .25-1 .0 mg · mL -1 for acetone (r=0 .999 8) ,and 0 .0445-0 .178 mg · mL -1 for toluene (r=0 .999 6) .The average recoveries were 100 .3% and 99 .9% ,RSDs were 1 .8% and 1 .3% ,respectively .Conclusion The methods were proved to be accurate and sensitive ,and can be used for the detec-tion of residual solvents in miconazole nitrate .