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頂空氣相色譜法測(cè)定帕利哌酮中的溶劑殘留量

發(fā)布時(shí)間:2018-11-28 13:54
【摘要】:目的建立頂空毛細(xì)管柱氣相色譜法測(cè)定帕利哌酮中的溶劑殘留量。方法以Agilent DB-624(30 m×530μm,3μm)柱為色譜柱,以氮?dú)鉃檩d氣,以氫火焰離子化檢測(cè)器檢測(cè),以N,N-二甲基乙酰胺為溶劑,采用程序升溫模式檢測(cè)帕利哌酮原料藥中甲醇、乙酸乙酯、二氯甲烷和三乙胺的殘留量。結(jié)果 4種揮發(fā)性有機(jī)溶劑均達(dá)到基線分離,在考察的質(zhì)量濃度內(nèi)線性良好(r≥0.999 0),平均回收率分別為103.1%、101.9%、101.3%和100.8%,RSD分別為2.9%、2.8%、3.3%和6.2%(n=9)。結(jié)論該方法操作簡(jiǎn)單、快速、靈敏、可靠,可用于帕利哌酮原料藥中4種有機(jī)溶劑殘留量測(cè)定。
[Abstract]:Objective to establish a headspace capillary gas chromatographic method for the determination of solvent residues in peridol. Methods Agilent DB-624 (30 m 脳 530 渭 m) column was used as chromatographic column, nitrogen as carrier gas, hydrogen flame ionization detector as detector, Nn- dimethyl acetamide as solvent, and temperature programmed mode for the determination of methanol in parpiperidone raw drug. Residues of ethyl acetate, dichloromethane and triethylamine. Results all of the four volatile organic solvents reached the baseline separation. The internal linearity of the four volatile organic solvents was good (r 鈮,

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