Kalman Andras, Mujahid Claudia, Mottier Pascal, Heudi Olivier
Department of Quality Assurance, Nestlé Research Center, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
Rapid Commun Mass Spectrom. 2003;17(7):723-7. doi: 10.1002/rcm.970.
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.
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。