LC/MSによるポリソルベート類の分析

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  • Qualitative analysis of polysorbates using liquid chromatography-mass spectrometry
  • LC MS ニ ヨル ポリソルベートルイ ノ ブンセキ

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In our previous study, we reported a rapid screening test method of polysorbates (PSs) using TLC. Although the method is useful in terms of obtaining characteristic spot pattern of PSs, it is impossible to discriminate each polysorbate (PS20, 40, 60, 80, 65 or 85) and to identify the molecular species in PSs. Thus we developed a new qualitative analytical method of PSs using LC/MS. PSs were separated on a YMC pack C8 column (150 mm × 2.0 mm I.D., 5 μm, 30 nm) by a gradient elution with a mixture of water-methanol containing 0.1% formic acid. PSs were analyzed in selected ion monitoring (SIM) mode, with Na+ adducts produced by electrospray ionization. Selected ion was calculated from the molecule consisting of Na+ adducts of 20 oxyethylene (EO) sorbitan (So) mono-, di-, or tri-ester of fatty acids (FA) (So-EO(20)-FA(1〜3)), respectively. the SIM peak of each PS was eluted at different retention time by constituent FA and esterification degree of PS and the PS with different length of EO (12〜35) was found in each SIM peak. Using the method we tried to identify the molecular species in the spots obtained by TLC analysis of PS40. Two major spots of TLC prepared by preparative thin layer chromatography (PTLC) were revealed to contain So-EO(20)-monopalmitate or So-EO(20)-dipalmitate by LC/MS. We also analyzed the extract from cocoa mix containing PS60 in SIM mode by LC/MS and found that it contained So-EO(20)-monostearate, tristearate and monopalmitate, the constituents of PS60. These results show that LC/MS analysis in SIM mode using Na+ adducts of So-EO(20)-FA(1〜3) as selected ions is useful not only for the analysis of compositional profile of PS itself, but for qualitative analysis of PS in food.

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