【摘要】：目的:采用色譜-質(zhì)譜聯(lián)用技術(shù)對西洛他唑有關(guān)物質(zhì)進行結(jié)構(gòu)鑒定。方法:采用Waters XTerra RP-8(100 mm×4.6mm,3.5μm)色譜柱串聯(lián)Agilent Eclipse XDB-C8(12.5 mm×4.6 mm,5μm)保護柱,以水-乙腈為流動相梯度洗脫,流速為1.0 m L·min-1,檢測波長為254 nm,對西洛他唑有關(guān)物質(zhì)進行分離;采用電噴霧正離子化的方法,通過飛行時間質(zhì)譜(TOF)測定一級質(zhì)譜精確質(zhì)量,三重四極桿/線性離子阱質(zhì)譜(Q-TRAP)掃描二級與三級質(zhì)譜,并進行結(jié)構(gòu)解析。飛行時間質(zhì)譜(TOF)和三重四極桿/線性離子阱質(zhì)譜(Q-TRAP)的噴霧電壓、霧化氣壓力、去溶劑溫度依次分別為4 k V和5.5 k V、240 k Pa和275 k Pa、350℃和480℃。結(jié)果:西洛他唑與其有關(guān)物質(zhì)分離良好,檢測出8個有關(guān)物質(zhì),其中4個尚未見文獻報道,并綜合分析鑒定了有關(guān)物質(zhì)結(jié)構(gòu)。它們大部分具有6-[4-(1-環(huán)己基-1H-戊四唑-5-基)丁氧基-2(1H)-喹諾酮結(jié)構(gòu),制劑中有關(guān)物質(zhì)狀態(tài)與原料藥中的相似。結(jié)論:色譜-質(zhì)譜聯(lián)用技術(shù)能有效地鑒定西洛他唑中有關(guān)物質(zhì),為其工藝和質(zhì)量控制提供參考依據(jù)。
[Abstract]:Objective: to identify the structure of cilostazol related substances by chromatography-mass spectrometry. Methods: Waters XTerra RP-8 (100 mm 脳 4.6 mm, 3.5 渭 m) column was used in series Agilent Eclipse XDB-C8 (12.5 mm 脳 4.6 mm, 5 渭 m). The mobile phase was eluted with water-acetonitrile as mobile phase, and the flow rate was 1.0 mL 路min-1. The detection wavelength was 254 nm, for the separation of cilostazol related substances. The accurate mass of primary mass spectrometry was determined by time-of-flight mass spectrometry (TOF) by electrospray positive ionization method. Triple quadrupole / linear ion trap mass spectrometry (Q-TRAP) was scanned for secondary and tertiary mass spectrometry, and the structure of the mass spectrometry was analyzed. The spray voltage, atomization pressure and solvent removal temperature of time-of-flight mass spectrometry (TOF) and triple quadrupole / linear ion trap mass spectrometry (Q-TRAP) are 4kV and 5.5kV, 240k Pa and 275k Pa,350 鈩，

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