【摘要】：目的:建立高效液相色譜-線性離子阱質(zhì)譜法分離鑒定瑞舒伐他汀藥物中間體N-[5-腈基-4-(4-氟苯基)-6異丙基嘧啶-2-]-N-甲基甲磺酰胺中的有關(guān)雜質(zhì),并探討這些雜質(zhì)的質(zhì)譜裂解規(guī)律。方法:采用Cortecs C18色譜柱(100 mm×2.1 mm,2.7μm),以乙腈-0.1%甲酸溶液為流動(dòng)相,進(jìn)行梯度洗脫,流速為0.25 m L·min-1,柱溫35℃,檢測(cè)波長(zhǎng)為242 nm,電噴霧離子化正負(fù)2種離子模式掃描。結(jié)果:中間體與各已知雜質(zhì)均分離良好,根據(jù)一級(jí)和多級(jí)質(zhì)譜信息,共鑒定出7種雜質(zhì),包括對(duì)甲基苯磺酸、4-(4-氟苯基)-2-羥基-6-異丙基-5-氰基-嘧啶、4-(4-氟苯基)-2-氨基-6-異丙基-5-氰基-嘧啶、5-氰基-6-(4-氟苯基)-4-異丙基-2-N-甲磺酰胺嘧啶-1-N-氧化物、4-(4-氟苯基)-2-甲氨基-6-異丙基-5-氰基-嘧啶、中間體的氯代產(chǎn)物和5-甲酸內(nèi)酯化產(chǎn)物。雜質(zhì)類(lèi)型主要為氧化、降解產(chǎn)物及合成副產(chǎn)物。結(jié)論:本法分析結(jié)果為有關(guān)雜質(zhì)確證提供分析方法,為瑞舒伐他汀合成中的質(zhì)量控制提供指導(dǎo)。
[Abstract]:Objective: to establish a high performance liquid chromatography-linear ion trap mass spectrometry for the separation and identification of the drug intermediate N- [5- nitrilyl-4- (4-fluorophenyl) -6-isopropylpyrimidine-2-] -N-methylmethanesulfonyl Related impurities in amine, The law of mass spectrometry cracking of these impurities was discussed. Methods: a Cortecs C18 column (100 mm 脳 2. 1 mm,2.7 渭 m),) with acetonitrile-0.1% formic acid solution as mobile phase was used for gradient elution. The flow rate was 0.25 mL min-1, at 35 鈩，

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