液相色谱-同位素稀释质谱法准确测定人血清中葡萄糖含量

以D-¹³C₆]葡萄糖标记物作为内标，用高效液相色谱 串联质谱法测定血清中的葡萄糖含量。向室温平衡后的血清样品中加入葡萄糖标记物，用乙醇沉淀蛋白，低温离心去除蛋白，上清液过0.22 μm有机滤膜。采用LC/MS电喷雾离子源（ESI），正离子模式，选择离子监测模式进行检测。方法的线性相关系数R²=0.999 5，加标回收率为100.1%~102.8%，检出限为8 μg/kg，相对标准偏差0.49%。该方法的样品前处理简单，测定准确高、精密度好，可用于血清中葡萄糖含量的高准确度定值。

Accurate Determination of Serum Glucose by Liquid Chromatography-Isotope Dilution Mass Spectrometry

A high performance liquid chromatography tandem mass spectrometric method was established for the determination of glucose concentration in serum with the aid of D-¹³C₆]glucose internal standard. D-¹³C₆]glucose was added to the serum sample in balance at room temperature. Then the protein was precipitated and extracted in anhydrous ethanol with centrifugation at low temperature. The supernatant was filtered through a 0.22 μm syringe filter into HPLC vials. Identification was achieved by electro-spray ionization (ESI) in positive mode using SIM mode. The calibration curve of glucose showed good linearity with correlation coefficient of R²=0.999 5, recoveries of spiked samples were in the range 100.1% to 102.8%, the detection limit of the method was 8 μg/kg (S/N=3), and the relative standard derivations were 0.49%. The established method is simple, accurate and precise, is appropriate for the determination of serum glucose with great accuracy.