邻苯二甲醛柱前衍生法测定食品中盐酸氨基葡萄糖的含量

Determination of Glucosamine Hydrochloride in Food by Pre-Column Derivatization of O-Phthalaldehyde

目的:建立邻苯二甲醛(OPA)柱前衍生法测定食品中盐酸氨基葡萄糖含量的分析方法。方法:取样品加入约40 mL水,超声处理30 min,用水定容至50 mL,用0.45μm滤膜过滤,经SHIMAZDU ODS-SP(4.6 mm×150 mm,5μm)分离,以0.68%醋酸缓冲液:甲醇(80:20,v:v)为流动相等度洗脱,流速1.0 mL/min,柱温35℃,进样量5μL,二极管阵列检测器340 nm波长采集数据,外标法定量。结果:盐酸氨基葡萄糖在10~1000 mg/L浓度范围内线性良好,相关系数R2为0.9995,3个浓度水平的加标回收率在91.1%~95.60%,相对标准偏差(n=6)为0.84%~1.10%,精密度的相对标准偏差(n=6)为0.61%,方法检出限为0.0050 g/100 g,定量限为0.0125 g/100 g。结论:该方法操作简便、灵敏度高,具有良好的准确度和精密度,适用于食品中盐酸氨基葡萄糖含量的测定。

Objective:To establish an analytical method for the determination of glucosamine hydrochloride content in food by pre-column derivatization of o-phthalaldehyde(OPA).Methods:Samples were filled in about 40 mL water and sonicated for 30 min.Then more water needed to be filled into the volumetric flask to meet 50 mL,then filtered with a 0.45μm membrane.The filtrate was separated by SHIMAZDU ODS-SP(4.6 mmx150 mm,5μm)and eluted with 0.68%acetic acid buffer:methanol(80:20,v:v)as flow equality at a flow rate of 1.0 mL/min and column temperature of 35,and injection volume of 5μL.The data were collected at 340 nm wavelength by diode array detector,and quantified by external standard method.Results:Glucosamine hydrochloride was linear in the range of 10~1000 mg/L concentration,and the correlation coefficient was 0.9995.The standard recovery of three concentration levels was between 91.1%~95.60%,with relative standard deviations at 0.84%~1.10%(n=6).The relative standard deviation(n=6)of precision was 0.61%.The detection limit of the method was 0.0050 g/100 g,and the quantitative limit was 0.0125 g/100 g.Conclusion:This method is easy to operate,high sensitivity,good accuracy and precision.It is suitable for the determination of glucosamine hydrochloride content in food.