摘要
建立了超高效合相色谱-质谱(UPC^2-MS)快速分析3种单甘酯乳化剂(单油酸甘油酯、单亚油酸甘油酯、单硬脂酸甘油酯)中单棕榈酸甘油酯、单硬脂酸甘油酯、单油酸甘油酯和单亚油酸甘油酯等4种主要的单甘酯的方法,并比较了这3种不同类别的乳化剂中此4种单甘酯的含量差异。采用正己烷/异丙醇(7:3,V/V)直接溶解样品,以ACQUITY UPC^2 BEH 2-EP色谱柱(100 mm×2.1 mm,1.7μm)为分析柱,以超临界CO_2-甲醇/乙腈(1:1,V/V)为流动相进行梯度洗脱,流速为1.0 mL/min。在电喷雾正离子模式下进行分析,外标法定量。结果表明:单棕榈酸甘油酯、单硬脂酸甘油酯、单亚油酸甘油酯在0.20~50mg/L范围内具有良好线性,单油酸甘油酯在0.25~62.5 mg/L范围内具有良好的线性(相关系数不小于0.9983);定量限(S/N≥10)为0.018~0.046 mg/L;在3个加标水平下,样品的回收率在88.0%~110.5%,相对标准偏差为1.1%~4.1%。本方法简单、快速、分离效果好,无需对单甘酯样品进行衍生化,为乳化剂中单甘酯的含量分析提供了一种新的色谱技术手段。
A fast analytical monoglycerides, including method was developed for the determination of main composition of fatty acid monopalmitin, monostearin, monoolein and monolinolein, in monoglycerede emulsifiers by ultra-performance convergence chromatography-mass spectrometry. Their contents were compared in the 3 emulsifiers from different sources. The sample was directly dissolved with n-hexane/isopropanol （7：3, /V） The chromatographic separation was performed on the ACQUITY UPC2 BEH 2-EP column （2.1 mm×100 mm, 1.7 μm） using the mobile phases of carbon dioxide and methanol/acetonitrile （1：1, V/V） solution with gradient elution. The separated compounds were detected by MS detector in positive electrospray ionization （ESI＋） and quantified by external standard method. The results showed that the calibration curves of monopalmitin, monostearin, monoolein and monolinolein were linear in the range of 0.20-50 mg/L, 0.20 - 50 mg/L, 0.25-62.5 mg/L and 0.20 - 50 mg/L, respectively, with correlation coefficients not less than 0. 9983. The limits of quantification （ S/N≥10） of the four fatty acid monoglyeerides were 0. 018-0.046 mg/L. The average recoveries for the four monoglycerides at three spiked levels were 88.0%-110.5% with relative standard deviations of 1. 1%-4. 1%. The proposed method showed high performance, good selectivity and fast analysis for the underivatized monoglyceride samples. It would provide a new chromatograohic technology for the content analysis of monoglvcerides in the emulsifier.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2016年第2期281-288,共8页
Chinese Journal of Analytical Chemistry
基金
国家科技支撑计划项目(Nos.2012BAE07B00
2014BAE13B02)资助~~
关键词
超高效合相色谱-质谱法
单甘酯
乳化剂
未衍生化
Ultra-performance convergence chromatography-mass spectrometry
Fatty acid monoglyceride
Emulsifier
Underivatization
