本文選題：氫溴酸右美沙芬　切入點(diǎn)：雜質(zhì)檢測　出處：《藥物分析雜志》2015年07期

【摘要】：目的:建立氫溴酸右美沙芬有關(guān)物質(zhì)的檢查方法。方法:采用比旋度法控制氫溴酸右美沙芬的左旋異構(gòu)體雜質(zhì),采用HPLC法測定其他有關(guān)物質(zhì)。色譜條件:采用Agilent Zobax SB-C18色譜柱(4.6 mm×250 mm,5μm),以含20 mmol·L-1十二烷基硫酸鈉的乙腈-水(600∶400)溶液(用冰醋酸調(diào)節(jié)p H至2.0)為流動相,流速1.0m L·min-1,檢測波長280nm,柱溫30℃,進(jìn)樣量20μL。結(jié)果:比旋度法能較好控制左美沙芬的限量,3批樣品的測定結(jié)果均為+25.6°。在所采用的液相色譜條件下,氫溴酸右美沙芬與各雜質(zhì)均可良好分離;N,N-二甲基苯胺、雜質(zhì)Ⅰ、雜質(zhì)Ⅱ、3-甲氧基-10-羰基-17-甲基嗎啡喃、N-氧化鹽酸右美沙芬、氫溴酸右美沙芬和3-甲氧基嗎啡喃質(zhì)量濃度分別在0.84~26.83μg·m L-1(r=0.999 9)、0.67~21.70μg·m L-1(r=0.999 9)、0.61~19.64μg·m L-1(r=0.999 9)、0.67~21.35μg·m L-1(r=1.000 0)、0.67~21.45μg·m L-1(r=0.999 6)、0.66~21.03μg·m L-1(r=0.999 9)和0.63~20.18μg·m L-1(r=1.000 0)范圍內(nèi)與峰面積呈良好的線性關(guān)系,其最低檢測限分別為3、7、6、0.3、7、7和6 ng;3批樣品中雜質(zhì)Ⅰ、雜質(zhì)Ⅱ、3-甲氧基-10-羰基-17-甲基嗎啡喃及N-氧化鹽酸右美沙芬均未檢出,3-甲氧基嗎啡喃的量分別為0.05%、0.05%、0.03%,最大單個未知雜質(zhì)量分別為0.01%、0.01%、0.12%,雜質(zhì)總量分別為0.07%、0.07%、0.15%。結(jié)論:本法經(jīng)方法學(xué)驗(yàn)證可用于氫溴酸右美沙芬的有關(guān)物質(zhì)檢測和質(zhì)量控制。
[Abstract]:Objective: to establish a method for the determination of related substances of dextromethorphan hydrobromide. Methods: the levoisomer impurity of dextromethorphan hydrobromide was controlled by specific curl method. Determination of other related substances by HPLC. Chromatographic conditions: a Agilent Zobax SB-C18 column of 4.6 mm 脳 250mm ~ 5 渭 m ~ (-1) with acetonitrile-water (600: 400) solution containing 20 mmol L-1 sodium dodecyl sulfate (adjusted by glacial acetic acid to pH 2.0) as mobile phase, The flow rate was 1.0 mL 路min -1, the detection wavelength was 280 nm, the column temperature was 30 鈩，

本文編號：1690152