【摘要】：目的:建立測定鹽酸倍他司汀片中乙烯吡啶、2-羥乙基吡啶、N-甲基-2吡啶乙胺等有關物質的檢查方法。方法:采用高效液相色譜法,以十八烷基硅烷鍵合硅膠為填充劑,以緩沖液(稱取醋酸銨0.69 g,用1 000 m L水溶解,以冰醋酸調節(jié)p H至4.7后,再加4.43 g十二烷基硫酸鈉溶解,脫氣)-乙腈(60∶40)為流動相,流速1.0 m L·min-1,檢測波長259 nm,柱溫40℃。結果:各雜質與主成分能完全分離,乙烯吡啶、2-羥乙基吡啶、N-甲基-2吡啶乙胺最低檢測限(S/N=3)分別為0.4、0.4、4 ng,回收率分別為97.9%、98.1%、101.7%,濃度與峰面積均呈線性(r0.999)。4個生產(chǎn)企業(yè)119批樣品檢驗,共檢出已知雜質2個(2-羥乙基吡啶、N-甲基-2吡啶乙胺)及未知雜質6個,各批次間檢查的雜質個數(shù)及雜質量不同:2-羥乙基吡啶、N-甲基-2吡啶乙胺含量分別為0.005%~0.47%、0.040%~1.26%,總雜質量在0.2%~5.3%范圍內(nèi)。結論:本文建立的方法符合方法學驗證要求,可用于鹽酸倍他司汀有關物質檢查。根據(jù)樣品檢測結果,建議將總雜質量定為2%。
[Abstract]:Objective: to establish a method for the determination of ethylpyridine, 2-hydroxyethylpyridine, N-methyl-2-pyridylethylamine and other related substances in Betastine Hydrochloride tablets. Methods: high performance liquid chromatography (HPLC) with octadecyl silane bonded silica gel as filler, buffer solution (ammonium acetate 0.69 g, dissolved in water of 1 000 mL), and acetic acid (acetic acid) were used to regulate pH to 4.7. The mobile phase was composed of 4.43 g sodium dodecyl sulfate dissolved and degassed) -acetonitrile (60:40). The flow rate was 1.0 mL min-1, and the column temperature was 40 鈩，

本文編號：2405735