通信作者:[email protected][中文文摘]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.[英文文摘].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 HPLC 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 0.8mL/min,and the injection volume of 10μL.This HPLC process was completed within 10 min.The resolution of GAH and GN was 2.32when the evaporation temperature of NQAD was 55℃and the pressure was 200kPa.The detection limit was 16ng for GAH and 8ng for GN,and the quantitation limit was 50ng for GAH and 24ng for GN.GAH showed a good linearity in the range of 10.03~2005.20μg/mL (r=0.999 5,)and the linearity range for GN was 10.18~2036.80μg/mL(r=0.9999,).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 HPLCNQAD
method was a reliable,quick and simple method for the detection of GAH and GN.海洋公益性专项(201005022
