CAJ | 학술논문

目的：建立盐酸普拉克索中5种残留溶剂的测定方法。方法采用顶空进样毛细管气相色谱法, FID检测器,应用DB624毛细管柱,柱温采取程序升温,初始温度50℃,保持10 min,再以15℃·min-1的速率升至250℃,保持2 min,测定盐酸普拉克索原料药中乙醇、乙醚、二氯甲烷、乙酸乙酯和四氢呋喃的残留量。结果各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r为0.9979~0.9999,平均回收率为97.24%~102.24%(RSD为0.98%~1.82%,n=9)。结论本方法符合方法学验证要求,可用于盐酸普拉克索原料药中残留有机溶剂的检测。
목적：건립염산보랍극색중5충잔류용제적측정방법。방법채용정공진양모세관기상색보법, FID검측기,응용DB624모세관주,주온채취정서승온,초시온도50℃,보지10 min,재이15℃·min-1적속솔승지250℃,보지2 min,측정염산보랍극색원료약중을순、을미、이록갑완、을산을지화사경부남적잔류량。결과각유궤용제균능득도유효분리,재소고찰적농도범위내선성관계량호,r위0.9979~0.9999,평균회수솔위97.24%~102.24%(RSD위0.98%~1.82%,n=9)。결론본방법부합방법학험증요구,가용우염산보랍극색원료약중잔류유궤용제적검측。
Objective To establish a method for the content determination of the five residual organic solvents in Pramipexole Hydrochloride raw materials.Methods Headspace GC was adopted to determinate alcohol,ether,dichloromethane,ethyl acetate and tetramethylene oxide in Pramipexole Hydrochloride raw materials.FID detector, DB624 capillary column and programmable temperature were applied, the temperature was initially kept at 50 ℃ for 10 minutes,then raised to 250 ℃ at the rate of 15 ℃·min-1 and kept for 2 minutes.Results Five residual solvents were completely separated with good linear relationships (0.9979-0.9999).The average recovery rates were in the range of 97.24%-102.24% (RSD0.98%-1.82%,n=9 ).Conclusion The established method was in line with the requirements of methodology validation,which can be used for the quality control of the residual organic solvents in Pramipexole Hydrochloride raw materials.