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液相色谱结合大气压化学电离质谱法测定婴儿食品中的α-生育酚

Determination of alpha-tocopherol in infant foods by liquid chromatography combined with atmospheric pressure chemical ionisation mass spectrometry.

作者信息

Kalman Andras, Mujahid Claudia, Mottier Pascal, Heudi Olivier

机构信息

Department of Quality Assurance, Nestlé Research Center, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.

出版信息

Rapid Commun Mass Spectrom. 2003;17(7):723-7. doi: 10.1002/rcm.970.

Abstract

A novel, sensitive and specific method for the quantification of alpha-tocopherol in two infant foods (milk and cereals) using liquid chromatography on-line with positive atmospheric pressure chemical ionisation mass spectrometry detection (LC/APCI-MS) has been developed. The samples were first saponified in order to eliminate fats and to transform tocopherol esters into free tocopherol, followed up by a liquid-liquid extraction of the analyte in petroleum benzine/diisopropyl ether (75:25, v/v) prior to injection onto the LC system. For the quantification, deuterium-labelled tocopherol was used as internal standard and the samples were monitored in selected ion monitoring (SIM) mode. Calibration curves between 1-40 microg/mL of alpha-tocopherol showed a good linear correlation (r(2) = 0.99994), and the detection limit was determined to be 2.5 ng/mL. The within-day and between-day precision were determined for several dietetic infant formulae and certified reference samples, and found to be below 3.5%. The accuracy determined on a Nestlé reference sample (milk powder) was calculated to be 115.2 +/- 1.2%, which confirms the robustness of the proposed method. This study shows that single quadrupole LC/MS can be applied for the quantification of vitamins in food and the method offers better sensitivity and selectivity than traditional method such as LC-UV. This would simplify the preparation of the food samples and consequently enhance the vitamin analysis throughput in the food area.

摘要

已开发出一种新颖、灵敏且特异的方法,用于使用液相色谱在线结合正大气压化学电离质谱检测(LC/APCI-MS)对两种婴儿食品(牛奶和谷物)中的α-生育酚进行定量。首先将样品皂化以去除脂肪并将生育酚酯转化为游离生育酚,然后在注入LC系统之前,在石油醚/二异丙醚(75:25,v/v)中对分析物进行液-液萃取。为了进行定量,使用氘标记的生育酚作为内标,并在选择离子监测(SIM)模式下监测样品。1-40μg/mL的α-生育酚校准曲线显示出良好的线性相关性(r(2)=0.99994),检测限确定为2.5ng/mL。对几种婴儿配方食品和有证参考样品测定了日内和日间精密度,发现均低于3.5%。在雀巢参考样品(奶粉)上测定的准确度经计算为115.2±1.2%,这证实了所提出方法的稳健性。本研究表明,单四极杆LC/MS可用于食品中维生素的定量,并且该方法比传统方法如LC-UV具有更好的灵敏度和选择性。这将简化食品样品的制备,从而提高食品领域维生素分析的通量。

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