本文選題：鹽酸多西環(huán)素　切入點(diǎn)：在線脫鹽-高效液相色譜-離子阱-飛行時(shí)間質(zhì)譜法　出處：《中國(guó)藥學(xué)雜志》2015年23期

【摘要】：目的應(yīng)用在線脫鹽-高效液相色譜-離子阱-飛行時(shí)間質(zhì)譜(2D-LC-IT-TOF/MS)法鑒定鹽酸多西環(huán)素片在藥典條件下檢出的有關(guān)物質(zhì)結(jié)構(gòu),并推斷鹽酸多西環(huán)素在溶液狀態(tài)下的降解途徑。方法 LC 1 stD色譜條件:InertSustain~(TM)C_(18)(4.6 mm×150 mm,5μm)色譜柱,醋酸鹽緩沖液[0.25 mol·L~(-1)醋酸-0.1 mol·L~(-1)EDTA鈉鹽-三乙胺(100:10:1),用醋酸或氨水調(diào)節(jié)pH值至8.8]-乙腈(85:15)為流動(dòng)相進(jìn)行等度洗脫;LC 2ndD色譜條件:InertSustain~(TM)C_(18)(2.1 mm×50 mm,2μm)色譜柱,0.1%甲酸冰溶液為流動(dòng)相A,0.1%甲酸福乙睛為流動(dòng)相B,進(jìn)行梯度洗脫;質(zhì)譜條件:ESI正負(fù)離子同時(shí)檢測(cè),霧化氣流速1.5L·min~(-1),干燥氣流速10 L·min~(-1)脫溶劑管溫度200℃。根據(jù)多級(jí)質(zhì)譜信息來(lái)推定藥典條件下檢出的有關(guān)物質(zhì)結(jié)構(gòu)和強(qiáng)制降解溶液中產(chǎn)生的雜質(zhì)結(jié)構(gòu)。結(jié)果在鹽酸多西環(huán)素片中共檢出8個(gè)有關(guān)物質(zhì)推定出其中4個(gè)含量大于0.1%的有關(guān)物質(zhì)的結(jié)構(gòu),分別為4-表多西環(huán)素、美他環(huán)素、β-多西環(huán)素、2-乙酰-6-脫碳酰胺多西環(huán)素。鹽酸多西環(huán)素溶液在堿性條件下易降解,生成脫酮基開環(huán)物;在高溫條件下容易產(chǎn)生4-表多西環(huán)素,并伴有少量4-表-6-表多西環(huán)素的生成;在酸性條件和光照條件下相對(duì)穩(wěn)定。結(jié)論建立的方法可用于鹽酸多西環(huán)素中雜質(zhì)的鑒定,為鹽酸多西環(huán)素的質(zhì)量控制與工藝優(yōu)化研究提供可靠的分析手段。
[Abstract]:Objective to identify the structures of related substances in doxycycline hydrochloride tablets under pharmacopoeia by on-line desalination, high performance liquid chromatography, ion trapping and time of flight mass spectrometry (TTOF / MS). The degradation pathway of doxycycline hydrochloride in solution was deduced. Methods the chromatographic conditions of LC 1 stD were as follows: 1. Acetic acid buffer solution [0.25 mol L~(-1)EDTA sodium salt-triethylamine 100: 10: 1, adjusted pH to 8.8 with acetic acid or ammonia] -acetonitrile: 8515) was used as mobile phase to perform isothermal elution with LC 2ndD chromatographic conditions:% InertCon sustained TMC182.1 mm 脳 50 mm ~ 2 渭 m) A 0.1% formic acid ice solution was used as mobile phase A0.1% formic acid as mobile phase. B was mobile phase B, gradient elution was carried out. Mass spectrometric conditions for simultaneous detection of positive and negative ions at 1: ESI level, The temperature of desolvent tube was 200 鈩，

本文編號(hào)：1667436