高效液相色谱-核粒子计数检测氨基葡萄糖类化合物  

Determination of Glucosamine Compounds by HPLC-nano-quantity Analyte Detector

作　　者：陈庆阳[1] 许建中[2] 夏金梅[2] 钟添华[2] 许晨[2] 

机构地区：[1]厦门大学化学化工学院,福建厦门361005 [2]国家海洋局第三海洋研究所,福建厦门361005

出　　处：《厦门大学学报（自然科学版）》2012年第6期1043-1046,共4页Journal of Xiamen University：Natural Science

基　　金：海洋公益性专项(201005022)

摘　　要：核粒子计数检测器是基于水凝聚激光计数专利技术(WCPC),对低紫外吸收的化合物有较强的优势.建立了高效液相色谱-核粒子计数检测器(HPLC-NQAD)检测D-氨基葡萄糖盐酸盐和N-乙酰-D-氨基葡萄糖的方法.采用AsahipakNH2(250mm×4.6mm,5μm)色谱柱,V(乙腈)∶V(0.5%三乙胺水溶液)=75∶25为流动相,流速为0.8mL/min,进样量为10μL,10min内完成检测.在NQAD蒸发管温度55℃、气体压力200kPa条件下,D-氨基葡萄糖盐酸盐与N-乙酰-D-氨基葡萄糖之间的分离度2.32,前者的检出限为16ng,定量限为50ng,后者的检出限为8ng,定量限为24ng.D-氨基葡萄糖盐酸盐在10.03～2 005.20μg/mL范围内线性回归相关系数为0.999 5,N-乙酰-D-氨基葡萄糖在10.18～2 036.80μg/mL范围内线性回归相关系数为0.999 9.检测D-氨基葡萄糖盐酸盐和N-乙酰-D-氨基葡萄糖的精密度实验的相对标准偏差(RSD)分别为1.53%和1.38%,平均回收率分别为100.18%和101.02%.该方法用于D-氨基葡萄糖盐酸盐和N-乙酰-D-氨基葡萄糖的检测,可靠、快速、简便.Nano quantity analyte detector （NQAD）, which was based on water condensation particle counter （WCPC） technology, was advantageous for detection of low UV-absorbing compounds. An effective HPI.C method with NQAD used for the detection of D-glucosamine hydrochloride （GAH） and N-acetyl-D glucosamine （GN） was developed. The separation was performed on a 250 mm × 4.6 mm NH2 column with a diameter of 5 μm （Asahipak）. Isocratic elution was conducted using acetonitrile/（0.5 % triethylamine） （75：25,by vol. ） with a flow rate of 0.8 mL/min,and the injection volume of 10 μL. This HPLC process was completed within 10 min. The resolution of GAH and GN was 2.32 when the evaporation temperature of NQAD was 55 C and the pressure was 200 kPa. The detection limit was 16 ng for GAH and 8 ng for GN,and the quantitation limit was 50 ng for GAH and 24 ng for GN. GAH showed a good linearity in the range of 10.03 - 2 005.20 μg/mL. （r=0. 999 5,） and the linearity range for GN was 10. 18- 036.80μg/mL （r=0. 999 9,）. The relative standard deviation of precision for GAH and GN were 1.53% and 1.38%,respectively. The average recovery rates of GAH and GN were 100. 18%and 101.02%,respectively. These results indicated that the HPLC- NQAD method was a reliable,quick and simple method for the detection of GAH and GN.

关 键 词：HPLC-NQAD D-氨基葡萄糖盐酸盐 N-乙酰-D-氨基葡萄糖 

分 类 号：O657.7[理学—分析化学]