为建立邻苯二胺(O-phenylenediamine,OPD)柱前衍生法测定蜂蜜中甲基乙二醛(Methylglyoxal,MGO)含量的分析方法.蜂蜜中的MGO用水提取,以OPD为柱前衍生剂,溶液用水系滤膜过滤,经Aglient ZORBAX Eclipse Plus C18(4.6 mm × 250 mm,5 μm)色谱柱分离,以乙腈∶水(30∶70,V∶V)为流动相等度洗脱,流速1.0 mL/min,柱温30 ℃,进样量10μL,二极管阵列检测器316 nm波长采集数据,外标法定量.结果表明,MGO在1～500 mg/L质量浓度范围内线性良好,相关系数R2为0.999 7,3个质量浓度水平的加标回收率为93.2％～107.9％,相对标准偏差(n=6)为1.25％～2.34％,精密度的相对标准偏差(n=6)为0.46％～0.73％,方法检出限为1.25 mg/kg,定量限为5mg/kg.该方法操作简便,灵敏度高,具有良好的准确度和精密度,适用于蜂蜜中MGO的定量分析.
Determination of Methylglyoxal in Honey by Pre-column Derivatization of O-Phenylenediamine
To establish an analytical method for the determination of methylglyoxal content in honey by pre-column derivatization of o-phenylenediamine(OPD).The MGO was extracted from honey by water,and OPD was used as a pre-column derivatization agent.The solution was filtered with a drainage filter membrane,after separated by Aglient ZORBAX Eclipse Plus C18(4.6 mm × 150 mm,5 μm),and eluted with acetonitrile∶water(30∶70,V∶V)as mobile phase.The flow rate was 1.0 mL/min,the column temperature was 30 ℃,and the injection volume was 10 μL.The data was collected at 316 nm wavelength by diode array detector,and quantified by external standard method.The results showed that MGO was linear in the range of 1～500 mg/L concentration,the correlation coefficient was 0.999 7,the standard recovery of three concentration levels was between 93.2％～107.9％,the relative standard deviation(n=6)was 1.25％～2.34％,the relative standard deviation(n=6)of precision was 0.46％～0.73％,the detection limit of the method was 1.25 mg/kg,and the quantitative limit was 5 mg/kg.This method was easy to operate,high sensitivity,good accuracy and precision,and was suitable for the quantitative analysis of MGO content in honey.
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