HPLC-ELSD测定磺丁基-β-环糊精钠中的有关物质

Determination of related substances in betadex sulfobutyl ether sodium by HPLC-ELSD

建立磺丁基-β-环糊精钠(SBE-β-CD)有关物质的HPLC-ELSD测定方法。采用CDScreen-IEC色谱柱(150mm×4mm,3μm)对有关物质倍他环糊精(β-CD)、4-羟基丁烷1-磺酸(HBSA)、双4磺丁基醚二钠(DBSA)进行定量分析,以0.4%三乙胺-甲酸缓冲液(pH4.5)和乙腈为流动相,采用梯度洗脱程序,流速为0.8mL/min,柱温25℃,漂移管温度40℃,载气(N2)压力3.5Pa。结果表明:在建立的色谱条件下,SBE-β-CD中三种有关物质分离度良好,β-CD、HBSA、DBSA线性范围分别为38.16~114.46μg/mL,R=0.999;39.14~117.42μg/mL,R=0.997;19.80~59.40μg/mL,R=0.999;检测限分别为9.54、5.87和9.96μg/mL,定量限分别为19.08、11.76和14.85μg/mL。该方法准确、灵敏、简便,可用于SBE-β-CD中有关物质的测定,为SBE-β-CD质量控制标准建立了快速有效的方法。

To establish a method to determine three substances in betadex sulfobutyl ether sodium by HPLC-ELSD. Methods:The CD-Screen-IEC chromatographic column(150 mm×4 mm,3 m)was used for quantitatively analysis of β-cyclodextrin,4-Hydroxybutane-1-sulfonic acid and bis(4-sulfobutyl)ether disodium. The gradient elution was made by 0.4% triethylamine-formic acid buffer(pH4.5). The flow rate was 0.8 mL/min,the column temperature was 25 ℃,the drift tube temperature was 40 ℃,and the carrier gas(N2)pressure was 3.5 Pa. Results:Under the above conditions,the three substances was well separated,and their linear ranges were 38.16 ~ 114.46μg/mL, R=0.999;39.14 ~ 117.42μg/mL,R=0.997;19.80 ~ 59.40μg/mL,R=0.999,respectively. The limit of detection was 9.54 g/mL,5.87 g/mL and 9.96 g/mL,respectively,and the limit of quantitation was 19.08,11.76 and 14.85 g/mL,respectively. Conclusion :This method is accurate,sensitive and simple. It provides a quick and effective method for the quality control of betadex sulfobutyl ether sodium.