CAJ | 학술논문

目的：建立高效液相色谱-四级杆/静电场轨道肼高分辨率质谱法直接测定蜂蜜中4-甲基咪唑和2-甲基咪唑的方法。方法用水溶解蜂蜜样品,经0.22μm粒径的微孔膜过滤后,采用Agilent HILIC Plus(2.1 mm ×100 mm,3.5μm)色谱柱进行分离,以体积比为8：2的乙腈与5 mmol/L乙酸铵水溶液为流动相进行等度洗脱。质谱采用正离子模式,在质荷比(m/z)50~400范围内通过高分辨质谱全扫描模式提取目标化合物的精确质量数。结果在本文建立的色谱条件下,4-甲基咪唑(4-MI)和2-甲基咪唑(2-MI)能够得到较好的分离,高分辨率质谱提取的质量准确度小于5×10-6(5 ppm)。该方法对4-MI的检测限可达50μg/kg,对2-MI的检测限可达25μg/kg。两种待测物质采用外标法定量,线性良好,相关系数均大于0.99。通过加标验证,在50、100和150μg/kg三个加标水平下,蜂蜜中4-MI和2-MI的平均回收率为73.2%~107.9%,相对标准偏差(RSD)小于9.7%。结论该方法样品处理过程简单,不使用有机溶剂,灵敏度高,适用于任何蜜种的测定,可以作为蜂蜜中是否掺入焦糖色素的检测方法。利用该方法对国内外各地区12个蜜种的30个蜂蜜样品进行检测,均未检出4-MI和2-MI。
목적：건립고효액상색보-사급간/정전장궤도정고분변솔질보법직접측정봉밀중4-갑기미서화2-갑기미서적방법。방법용수용해봉밀양품,경0.22μm립경적미공막과려후,채용Agilent HILIC Plus(2.1 mm ×100 mm,3.5μm)색보주진행분리,이체적비위8：2적을정여5 mmol/L을산안수용액위류동상진행등도세탈。질보채용정리자모식,재질하비(m/z)50~400범위내통과고분변질보전소묘모식제취목표화합물적정학질량수。결과재본문건립적색보조건하,4-갑기미서(4-MI)화2-갑기미서(2-MI)능구득도교호적분리,고분변솔질보제취적질량준학도소우5×10-6(5 ppm)。해방법대4-MI적검측한가체50μg/kg,대2-MI적검측한가체25μg/kg。량충대측물질채용외표법정량,선성량호,상관계수균대우0.99。통과가표험증,재50、100화150μg/kg삼개가표수평하,봉밀중4-MI화2-MI적평균회수솔위73.2%~107.9%,상대표준편차(RSD)소우9.7%。결론해방법양품처리과정간단,불사용유궤용제,령민도고,괄용우임하밀충적측정,가이작위봉밀중시부참입초당색소적검측방법。이용해방법대국내외각지구12개밀충적30개봉밀양품진행검측,균미검출4-MI화2-MI。
Objective A method of high performance liquid chromatography-quadrurpole/ electrostatic field orbitrap high resolution mass spectrometry (HPLC-Q/qrbitrap MS) was developed to determine 4-methylimidazole and 2-methylimidazole in honey.Methods The honey samples were diluted with deio-nized water, and then filtered by a polytetrafluoroethylene (PTFE) membrane with pore size of 0.22μm. The analytes were separated on an Agilent HILIC Plus (2.1 mm × 100 mm, 3.5μm) column through isocratic elu-tion with acetonitrile and 5 mmol/L of ammonium acetate aqueous solution (v:v, 8:2). Full scan experiments were performed over the range ofm/z 50~400 in positive mode to extract the accurate mass of analytes. Results Under the optimal condition, 4-methylimidazole (4-MI) and 2-methylimidazole (2-MI) were well separated, and the accuracy of extracted mass routinely detected was below 5×10-6. The detection limits for 4-MI and 2-MI were 50μg/kg and 25μg/kg, respectively. Good linearities were provided in their respective linear ranges with correlation coefficients higher than 0.99. The average recoveries at three spiked levels (50, 100 and 150μg/kg) were in the range of73.2 %~107.9 % and the relative standard deviations (RSDs) lower than 9.7 %.Conclusion The proposed method was simple, on use of organic solvents, sensitive, and can therefore meet the requirements of the determination of caramel color in all kinds of honey. The method was applied to 30 honey samples of 12 species from domestic and other countries. The results showed that neither 4-MI nor 2-MI was detected.