中文摘要：

采用柱前衍生高效液相色谱-电喷雾质谱法（HPLC-ESI-MS）测定了人血浆中的氨基葡萄糖浓度.该方法以氨基半乳糖为内标,用丙酮沉淀蛋白后,加入5μL三乙胺和10μL异硫氰酸苯脂后,在60℃的恒温水浴中反应1 h,用氮气吹干、流动相溶解后于离心机上以12 000 r/min离心5 min后进样20μL分析;以甲醇与水作流动相,经过Ultimate-XB C18柱（4.6 mm×250 mm,5μm,Welch Materials）在梯度模式下分离后1∶4分流,以0.2 mL/min的流速进质谱分析.实验结果表明：氨基葡萄糖的回归方程为Y=6.70×10-4X＋1.11×10-2（r2=0.996）,在0.10-5.00μg/mL范围内线性关系良好;最低定量限为0.10 mg/L;氨基葡萄糖和内标的萃取回收率分别为88.3%-92.1%和85.2%;日内、日间精密度的RSD值分别为〈6.0%、〈5.0%,稳定性的RSD〈7.5%.所建立的方法准确度好、灵敏度高、稳定性好,适合于血浆中的氨基葡萄糖的含量测定.

英文摘要：

A high performance liquid chromatography-electrospray ionization mass spectrometry（HPLC-ESI-MS） method with pre-column derivatization was established and validated for the determination of glucosamine in human plasma.In this paper D（＋）-Galactosamine was selected as internal standard（I.S.） for the quantification of target compound.Plasma sample were deproteinized by acetone,and the supernatant was transferred into a clean polyethylene tube,then 5 μL triethylamine and 10 μL phenylisothiocyanate was added,and allow them to react for 1 h in the constant temperature water bath about 60 ℃.After derivatization,the sample solution was dried by nitrogen,dissolved with mobile phase and centrifuged at 12 000 r/min for 5 min.The supernatant was transferred into separate vials;sequentially 20 μL was injected onto the column for analysis.The chromatographic separation was performed on an Ultimate-XB C18 column（4.6 mm×250 mm,5 μm,Welch Materials） with a mobile phase containing methanol and water eluting on the gradient mode.The outlet of column was splited by the ratio of 1∶4 and only 0.2 mL/min was delivered into the MS.The results showed equation of linear regression was Y=6.70×10-4X＋1.11×10-2（r2=0.996）which showed a good linearity in the range of 0.10~5.00 mg/L.The limit of quantification（LOQ） was 0.10 μg/mL.Extraction recoveries of glucosamine and I.S in plasma were 88.3%~92.1% and 85.2%,respectively.The coefficient variations were less than 6.0%,5.0%,and 7.5% for the precision of intra-day,inter-day and stability,respectively.The method with good accuracy,high sensitivity and good stability was applied to the determination of glucosamine in human plasma.