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Update of on-line coupled liquid chromatography – gas chromatography for the analysis of mineral oil hydrocarbons in foods and cosmetics
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2017-09-13 , DOI: 10.1016/j.chroma.2017.09.028
Maurus Biedermann , Celine Munoz , Koni Grob

On-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) is the most widely used method for the analysis of mineral oil hydrocarbons in food, food contact materials, tissues and cosmetics. With comprehensive two-dimensional gas chromatography (GCxGC), a tool became available for better establishing the elution sequence of the various types of hydrocarbons from the HPLC column used for isolating the mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH). The performance of a heavily used HPLC column with reduced retention for MOAH was investigated to improve the robustness of the method. Updates are recommended that render the MOSH/MOAH separation less dependent of the state of the HPLC column and more correct in cases of highly refined mineral oil products of high molecular mass. Cyclohexyl cyclohexane (Cycy), used as internal standard, turned out to be eluted slightly after cholestane (Cho); apparently the size exclusion effect predominates the extra retention by ring number on the 60 Å pore size silica gel. Hence, Cycy can be used to determine the end of the MOSH fraction. Long chain alkyl benzenes were eluted earlier than tri-tert. butyl benzene (Tbb). It is proposed to start the MOAH transfer immediately after the MOSH fraction and use a gradient causing breakthrough of dichloromethane (visible in the UV chromatogram) at a time suitable to elute perylene (Per) at the end of the fraction. In this way, a decrease in retention power of the HPLC column can be tolerated without adjustment of the MOAH fraction until some MOAH start being eluted into the MOSH fraction. This critical point can be checked either with di(2-ethylhexyl) benzene (DEHB) as a marker or the HPLC-UV chromatogram. Finally, based on new findings in rats and human tissues, it is recommended to integrate the MOSH and MOAH up to the retention time of the n-alkane C40.



中文翻译:

在线耦合液相色谱-气相色谱分析食品和化妆品中的矿物油烃的更新

在线耦合高效液相色谱-气相色谱-火焰电离检测(HPLC-GC-FID)是分析食品,食品接触材料,组织和化妆品中矿物油烃的最广泛使用的方法。借助全面的二维气相色谱仪(GCxGC),可以使用一种工具来更好地确定HPLC色谱柱中各种烃的洗脱顺序,该色谱柱用于分离矿物油饱和烃(MOSH)和矿物油芳烃(MOAH) 。为了提高方法的耐用性,研究了减少使用MOAH的保留量较高的HPLC色谱柱的性能。建议进行更新,以使MOSH / MOAH分离更不依赖HPLC色谱柱的状态,而对于高度纯化的高分子量矿物油产品,则更正确。用作内标的环己基环己烷(Cycy)在胆甾烷(Cho)之后被轻微洗脱;显然,在60孔径孔径的硅胶上,尺寸排阻作用优先于环数的额外保留。因此,Cycy可用于确定MOSH分数的结尾。长链烷基苯的洗脱早于三叔。丁基苯(Tbb)。建议在MOSH馏分之后立即开始MOAH转移,并使用适合于在馏分结束时洗脱per(Per)的时间使二氯甲烷穿透(在UV色谱图中可见)的梯度。通过这种方式,在不调整MOAH馏分的情况下,可以忍受HPLC色谱柱保留力的降低,直到某些MOAH开始被洗脱到MOSH馏分中为止。可以使用二(2-乙基己基)苯(DEHB)作为标记物或HPLC-UV色谱图检查该临界点。最后,根据在大鼠和人体组织中的新发现,建议将MOSH和MOAH整合到小鼠的保留时间之前。构烷烃C40。

更新日期:2017-09-13
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