摘要
建立了高效液相色谱法用于检测新西兰Manuka蜂蜜中的甲基乙二醛.将蜂蜜溶于水后加入邻苯二胺水溶液,在室温、避光条件下衍生化反应8h以上,产物过0.22 μm滤膜后用HPLC检测.以Kromasil反相色谱柱为分析柱;甲醇和0.1％ （v/v）乙酸水溶液为流动相,梯度洗脱;检测波长为318 nm;外标法定量.甲基乙二醛在1～50mg/L范围内线性良好,相关系数为0.999 9;检出限（S/N=3）为0.02 mg/L,定量限（S/N=10）为0.06 mg/L;在50、100、200 mg/kg添加水平下的回收率为98.3％～ 101.5％,相对标准偏差（n=5）小于5％;衍生化产物在24 h内稳定.实验结果表明,该方法前处理过程简单,具有良好的灵敏度、回收率和重复性,可用于新西兰Manuka蜂蜜的质量控制.该方法也适用于中国蜂蜜中甲基乙二醛的检测.
An HPLC method was developed for the determination of methylglyoxal in Manuka honey of New Zealand. The honey sample was dissolved in water and mixed with o-phenylene- diamine solution for derivatization. After the reaction for at least 8 h in the dark at room tem- perature, the solution was filtered with 0.22 ~m membrane and injected into an HPLC system for analysis. The separation was carried out on a Kromasil reversed phase column with gradient elution. The mobile phases were methanol and 0. 1% （v/v） acetic acid aqueous solution. The detection wavelength was 318 nm. The external standard method was used for quantitation. The linear range of methylglyoxal was 1-50 mg/L with a correlation coefficient of 0. 999 9. The LOD （ S/N = 3 ） and LOQ （ S/N= I 0） were 0.02 mg/L and 0.06 mg/L, respectively. The recoveries at the spiked levels of 50, 100, 200 mg/kg were 98.3%-101.5% and the RSDs （n= 5） were less than 5%. The derivative of methylglyoxal was stable within 24 h. The results showed that the pretreatment of this method is simple and the sensitivity, the recovery and repeatability are good. This method can be used for the quality control of Manuka honey of New Zealand, and also for the detection of methylglyoxal in Chinese honey.
出处
《色谱》
CAS
CSCD
北大核心
2014年第2期189-193,共5页
Chinese Journal of Chromatography
基金
国家质检总局科技计划项目(2013KJ40)
国家质检总局科技计划项目(2011IK209)
关键词
高效液相色谱
甲基乙二醛
Manuka
蜂蜜
high performance liquid chromatography （HPLC）
methylglyoxal （MGO）
Manuka
honey
