【摘要】：目的:制備鹽酸多西環(huán)素中國藥典2015年版(Ch P 2015)標準檢測的緊鄰主峰后雜質(zhì),并鑒定其結(jié)構(gòu)。方法:以鹽酸多西環(huán)素成鹽用母液為對象,采用室溫條件下半制備液相色譜分離純化雜質(zhì);色譜條件:采用Synergi C_(18)(50 mm×250 mm,10μm)色譜柱,以0.1%三氟乙酸水溶液(A)-0.1%三氟乙酸乙腈溶液(B)為流動相,線性梯度洗脫(A-B):0.0 min(85∶15)→40.0 min(60∶40)→40.5 min(85∶15)?50.0 min(85∶15),流速為80 m L·min~(-1);254 nm檢測收集目標組分,旋轉(zhuǎn)蒸發(fā)去除有機溶劑,冷凍干燥制得目標雜質(zhì);采用鹽酸多西環(huán)素Ch P 2015標準中有關(guān)物質(zhì)檢查的高效液相色譜法確證制得物質(zhì)為目標雜質(zhì)并采用歸一化方法測定其純度;采用光譜綜合分析等手段確證其結(jié)構(gòu)。結(jié)果:制得目標雜質(zhì)純度為98.7%,結(jié)構(gòu)確證為2-乙酰-2-脫氨甲酰多西環(huán)素(即EP 8.0中的鹽酸多西環(huán)素雜質(zhì)F),在有關(guān)物質(zhì)測定用供試品溶液中添加該雜質(zhì)后,多西環(huán)素后相鄰峰面積顯著增加。結(jié)論:鹽酸多西環(huán)素Ch P 2015標準檢測的緊鄰主峰后雜質(zhì)經(jīng)制備色譜分離并成功鑒定,該結(jié)論被Ch P 2015采用。
[Abstract]:Aim: to prepare doxycycline hydrochloride (Ch P 2015) and identify its structure. Methods: the impurities were separated and purified by semi-preparative liquid chromatography at room temperature, and the chromatographic conditions were as follows: Synergi C18 (50 mm 脳 250 mm,10 渭 m) column. Using 0.1% trifluoroacetic acid aqueous solution (A) -0.1% trifluoroacetic acid acetonitrile solution (B) as mobile phase, linear gradient elution (A-B) 0.0 min (85:15) 40.0 min (60:40) 40.5 min (85:15) 50.0 min (85:15), flow rate 80ml min~ (-1) 254nm detection and collection target group, rotating evaporation to remove organic solvent, The target impurity was prepared by freeze-drying, and the purity of the substance was determined by normalized method by high performance liquid chromatography (HPLC) about substance examination in Ch P 2015 standard of doxycycline hydrochloride. The structure was confirmed by means of spectral comprehensive analysis. Results: the purity of the target impurity was 98.7 and the structure was confirmed as 2-acetyl-2-decarbamicyloxycycline (F), the dopicycline hydrochloride impurity in EP 8.0, which was added to the sample solution for the determination of related substances. The area of adjacent peaks increased significantly after doxycycline. Conclusion: the impurities of doxycycline hydrochloride Ch P 2015 were separated by preparative chromatography and identified by Ch P 2015.
【作者單位】： 南京理工大學醫(yī)院;江蘇省食品藥品監(jiān)督檢驗研究院;中國藥科大學藥物化學教研室;常州制藥廠有限公司;中國醫(yī)藥城公共平臺服務(wù)中心;
【分類號】：R943;R927

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