Screening for mineral oil hydrocarbons in vegetable oils by silver ion-planar solid phase extraction.

Screening for mineral oil hydrocarbons in vegetable oils by silver ion-planar solid phase extraction.
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银离子平面固相萃取法筛选植物油中的矿物油烃

DOI:
10.1016/j.chroma.2021.462732
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发表时间:
2022
期刊:
Journal of chromatography. A
影响因子:
--
通讯作者:
C. Oellig
C. Oellig
中科院分区:
--
文献类型:
--
作者:
M. Wagner;C. Oellig

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植物油中矿物油烃的分析具有挑战性,尤其是矿物油芳香烃 (MOAH) 的分析,因为角鲨烯或 β-胡萝卜素等天然萜烯通常与 MOAH 馏分一起提取并干扰其检测。当应用最近开发的筛选方法通过平面固相萃取 (pSPE) 对植物油分析纸张和纸板中的矿物油饱和烃 (MOSH) 和 MOAH 时,天然萜烯预计会干扰 MOAH 分析。因此,本研究开发了一种采用银离子的 pSPE,称为银离子平面固相萃取 (Ag-pSPE)。人们发现用硝酸银(AgNO3)浸渍薄层可以非常成功地保留角鲨烯和β-胡萝卜素。皂化后植物油的 MOAH 分析显示出良好的重复性(相对标准偏差 (%RSD) <10%),在 4.5 mg/kg 的加标水平下回收率为 73.4–112.4% (n=4)。对于 MOSH 分析,在 Ag-pSPE 之前,使用氧化铝进行简单的固相萃取 (SPE) 净化,去除天然烷烃。当加标水平为 45.5 mg/kg 时,MOSH 的回收率为 55.3–84.5%,%RSD<11% (n=4)。 MOSH 的决策限和定量限分别为 7.2 和 22.2 ng/区,MOAH 的决策限和定量限分别为 1.1 和 3.4 ng/区,这与最近引入的 pSPE 方法相对应,因此表明分析物不受 HPTLC 板用 AgNO3 浸渍的影响。与 LC-GC 的方法比较显示 MOSH 的结果相似,而 Ag-pSPE 测定的 MOAH 的含量更高。
The analysis of mineral oil hydrocarbons in vegetable oils is challenging especially regarding the analysis of mineral oil aromatic hydrocarbons (MOAH) since native terpenes like squalene or β-carotene are usually extracted along with the MOAH fraction and interfere their detection. When applying a recently developed screening method for the analysis of mineral oil saturated hydrocarbons (MOSH) and MOAH in paper and cardboard by planar solid phase extraction (pSPE) to vegetable oils, native terpenes expectably interfered with MOAH analysis. Thus, an adaption of pSPE employing silver ions, named silver ion–planar solid phase extraction (Ag–pSPE), was developed in this study. Impregnation of thin-layers with silver nitrate (AgNO3) was found to be very successful in retaining squalene and β-carotene. MOAH analysis of vegetable oils after saponification showed good repeatability (relative standard deviation (%RSD) <10%) and recoveries of 73.4–112.4% at a spiking level of 4.5 mg/kg (n= 4). For MOSH analysis, a simple solid phase extraction (SPE) clean-up with aluminum oxide removed nativen-alkanes prior to Ag–pSPE. Recoveries for MOSH were 55.3–84.5% with %RSD<11% at a spiking level of 45.5 mg/kg (n= 4). Limits of decision and quantitation were at 7.2 and 22.2 ng/zone for MOSH and 1.1 and 3.4 ng/zone for MOAH, respectively, which corresponded to the recently introduced pSPE method, thus showing that analytes were not affected by the impregnation of HPTLC plates with AgNO3. The method comparison with LC–GC showed similar results for MOSH, while the amounts for MOAH determined by Ag–pSPE were higher.
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