【摘要】：目的建立HPLC法測(cè)定注射用脫氧核苷酸鈉和脫氧核苷酸鈉注射劑中的有關(guān)物質(zhì),并應(yīng)用LC-MS/MS法推測(cè)有關(guān)物質(zhì)結(jié)構(gòu)。方法采用HPLC法測(cè)定2種脫氧核苷酸鈉制劑中的有關(guān)物質(zhì)。色譜柱為Agilent Zorbax SAX柱(250 mm×4.6 mm,5μm),流動(dòng)相為濃度50 mmol·L-1的磷酸二氫鉀溶液(取6.80 g磷酸二氫鉀,加水800 m L,用磷酸調(diào)p H值至3.3,再加水稀釋至1 000 m L),流速為0.6 m L·min-1,柱溫為30℃,進(jìn)樣量為20μL,檢測(cè)波長(zhǎng)為258 nm。結(jié)果 2種脫氧核苷酸鈉制劑中脫氧核糖胞嘧啶核苷酸鈉(d CMP-Na)、脫氧核糖腺嘌呤核苷酸鈉(d AMP-Na)、脫氧核糖胸腺嘧啶核苷酸鈉(d TMP-Na)和脫氧核糖鳥嘌呤核苷酸鈉(d GMP-Na)分別與其相鄰色譜峰完全分離,測(cè)得的注射用脫氧核苷酸鈉中最大單個(gè)有關(guān)物質(zhì)百分含量均不大于2.0%,有關(guān)物質(zhì)總量均不大于4.0%。脫氧核苷酸鈉注射劑中最大單個(gè)有關(guān)物質(zhì)百分含量平均大于30%,而有關(guān)物質(zhì)總量更是達(dá)到79%以上。經(jīng)質(zhì)譜分析,推測(cè)注射用脫氧核苷酸鈉有關(guān)物質(zhì)為5-甲基胞嘧啶脫氧核糖核苷酸,脫氧核苷酸鈉注射劑有關(guān)物質(zhì)為胞嘧啶核糖核苷酸、尿嘧啶核糖核苷酸和鳥嘌呤核糖核苷酸。結(jié)論該方法簡(jiǎn)便,準(zhǔn)確,專屬性較好,適用于脫氧核苷酸鈉制劑的質(zhì)量分析,為脫氧核苷酸鈉制劑臨床用藥的安全性改善提供參考。
[Abstract]:Objective to establish a HPLC method for the determination of related substances in sodium deoxynucleotides and sodium deoxynucleotides for injection and to speculate the structure of related substances by LC-MS/MS method. Methods HPLC method was used to determine the related substances in two kinds of sodium deoxynucleotide preparations. The chromatographic column was Agilent Zorbax SAX column (250 mm 脳 4.6 mm,5 渭 m), mobile phase: 50 mmol L-1 potassium dihydrogen phosphate solution (6.80 g potassium dihydrogen phosphate, 800 mL water, adjusted pH value to 3.3 with phosphoric acid, diluted to 1 000 m L), flow rate of 0.6 mL min-1, at 30 鈩，

本文編號(hào)：2245098