UPLC-QDa测定乳果糖口服溶液中乳果糖及其有关物质含量

Determination of the Contents of Lactulose and Related Substances in Lactulose Oral Solution by UPLC-Qda

关键词:  乳果糖口服溶液|含量测定|有关物质|UPLC-QDa

Key words:  lactulose oral solution|content determination|related substances|UPLC-QDa

摘要:

目的 采用UPLC-QDa测定乳果糖口服溶液中乳果糖的含量及其有关物质塔格糖、果糖、半乳糖、依匹乳糖、乳糖的含量。方法 采用ACQUITY UPLC BEH Amide（2.1 mm×100 mm，1.7 μm）色谱柱，以水（含0.1%二乙胺，500 ng·mL^-1盐酸胍）和乙腈（含0.1%二乙胺，500 ng·mL^-1盐酸胍）为流动相，梯度洗脱，流速0.6 mL·min^-1，电喷雾离子化（ESI），负极性下SIR模式采集。结果 塔格糖、果糖、依匹乳糖、乳果糖的定量限分别为0.5，0.5，0.2，0.2 μg·mL^-1，乳糖和半乳糖的检测限分别为0.2，2 μg·mL^-1；塔格糖、果糖、半乳糖、依匹乳糖、乳果糖、乳糖分别在5.1~123.2，4.9~117.8，5.4~129.8，5.2~125.0，5.0~119.9和5.0~121.2 μg·mL^-1内呈良好的线性关系，r均 ≥ 0.995；平均加样回收率均为90%~107%（n=6）；方法仪器精密度良好，峰面积RSD均<2.8%（n=5）。2个不同厂家生产的乳果糖口服溶液中乳果糖的含量和有关物质塔格糖、果糖、半乳糖、依匹乳糖、乳糖的含量均符合中国药典2015年版规定，并与中国药典方法结果基本一致。结论 该方法可用于乳果糖口服溶液中乳果糖和有关物质含量的检测分析。

Abstract:

OBJECTIVE To establish UPLC-QDa for the content determination of lactulose and its related substances including tagatoes, fructose, galactose, epilactose, lactose in lactulose oral solution. METHODS ACQUITY UPLC BEH Amide column(2.1 mm×100 mm, 1.7 μm) was used for the separation with a mobile phase of water(containing 0.1% diethylamine and 500 ng·mL^-1 guanidine hydrochloride) and acetonitrile(containing 0.1% diethylamine and 500 ng·mL^-1 guanidine hydrochloride) at a flow rate of 0.6 mL·min^-1 in gradient elution mode. The method was developed at ESI(-) with SIR mode. RESULTS The limit of quantitation of tagatoes, fructose, epilactose and lactulose were 0.5, 0.5, 0.2 and 0.2 μg·mL^-1, respectively. The limit of detection of lactose and galactose were 0.2 and 2 μg·mL^-1, respectively. The linearity ranges of the tagatoes, fructose, galactose, epilactose, lactulose, lactose were 5.1-123.2, 4.9-117.8, 5.4-129.8, 5.2-125.0, 5.0-119.9 and 5.0-121.2 μg·mL^-1 respectively, with the excellent correlation coefficient(r ≥ 0.995). The average recoveries were 90%-107% (n=6). The instrument of methods had a good precision. The RSD of peak area were all < 2.8% for the six target compounds(n=5). The contents of lactulose and related substances in lactulose oral solution produced by two different manufacturers were all in accordance with the regulations of Chinese Pharmacopoeia 2015 Edition, and were basically consistent with the results of method in Chinese Pharmacopoeia. CONCLUSION The established method can be applied to the determination of the contents of lactulose and related substances in lactulose oral solution.