UPLC-MS/MS测定参芎葡萄糖注射液中阿拉伯糖、果糖、甘露糖和葡萄糖

Determination of Sugar,Fructose,Mannose and Glucose in Shenxiong Glucose Injection by UPLC-MS/MS

目的:建立超高效液相色谱-三重四级杆质谱联用仪(UPLC-MS/MS)法测定参芎葡萄糖注射液中阿拉伯糖、果糖、甘露糖、葡萄糖的含量测定方法,为科学评价参芎葡萄糖注射液的质量提供依据,为保障临床安全用药奠定基础。方法:采用国产GDX-403固相萃取柱净化,Waters ACQUITY UPLC BEH Xbridge Amide色谱柱(2.1 mm×100 mm,1.7μm),柱温35℃进行分析;[(0.1%氨水-乙腈)-(0.1%氨水-水)](85∶15)为流动相进行分离,流速0.3 mL·min-1,以超高效液相色谱-三重四级杆质谱联用仪(UPLC-MS/MS)测定参芎葡萄糖注射液中阿拉伯糖、甘露糖、果糖和葡萄糖含量。结果:建立了参芎葡萄糖注射液中阿拉伯糖、果糖、甘露糖、葡萄糖的含量测定方法,所测定的样品中和混合对照品中阿拉伯糖、果糖、甘露糖、葡萄糖相应的浓度范围与峰面积呈良好的线性关系,重复性、精密度良好,加样回收率分别为98.43%,102.13%,100.72%,101.75%,其RSD分别为2.4%和1.3%,3.1%,2.7%。5个批次参芎葡萄糖注射液中阿拉伯糖和甘露糖含量稳定。结论:该操作方法简便,专属性强,与总糖的含量测定相比更加科学稳定,可用于参芎葡萄糖注射液的质量控制。

Objective: To establish a method for determining arabinose,mannose,fructopyranose and amylaceum in Shenxiong glucose injection by UPLC-MS /MS,so as to provide the basis for the scientific evaluation of the quality of Shenxiong glucose injection,and lay a foundation for the safe use of drugs in clinic. Method: Domestic GDX-403 solid-phase extraction column was used to purify Waters ACQUITY UPLC BEH Xbridge Amide column ( 2. 1 mm × 100 mm,1. 7 μm) at the column temperature of 35 ℃,and the mobile phase was 0. 1% ammonia,0. 1% acetonitrile-0. 1% ammonia water and water 85 ∶ 15. The contents of arabinose,mannose, fructose and glucose in Shenxiong glucose injection were determined by UPLC-MS /MS with a flow rate of 0. 3 mL·min - 1 . Result: A method was established to determine arabinose,mannose, fructopyranose and amylaceum in Shenxiong glucose injection. The concentration range of arabinose,mannose,fructopyranose and amylaceum showed a good linear relationship with the peak area,with a good repeatability and precision. Recoveries were 98. 43%,102. 13%,100. 72%,101. 75%,and RSD were 2. 4%,1. 3%,3. 1%,2. 7%. Arabinose and mannose content were stable in five batches of Shenxiong glucose injection. Conclusion: The method is simple and specific. Compared with the determination of total sugar,the method is more scientific and stable,and can be used for the quality control of Shenxiong glucose injection.