超高效液相色谱-串联质谱法测定酒类中纽甜

Determination of Neotame in Alcoholic Drinks by Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了一种测定白酒、葡萄酒、黄酒、米酒以及果酒中纽甜含量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品水浴加热除酒精后经超纯水稀释,定容至一定体积,微孔滤膜过滤后直接进样,用超高效液相色谱-串联质谱分析,外标法定量。采用Waters BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm)为分析柱,乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,采用电喷雾电离源负离子模式监测。结果表明,纽甜在1~50 ng/mL的范围内线性关系良好(相关系数r=0.995),方法检出限0.05 mg/kg,基质加标回收率为76.90%~101.55%,相对偏差<8%,完全满足日常检测的要求。该检测方法前处理简单,测定快速、准确,灵敏度高,较为适合各种酒类中纽甜的快速筛查和定量分析。

A method for the determination of neotame in Baijiu, grape wine, yellow rice wine, rice wine and fruit wine by UPLC-MS/MS had been developed. Samples were heated by water bath for alcohol removal and then diluted to a certain volume with distilled water, then filtered through micro-porous membrane, and directly injected for testing by UPLC-MS/MS and by external standard method. The UPLC separation was performed on a Waters BEH C_（18） column（2.1 mm×50 mm, 1.7 μm）, and 0.1 %v/v acetic/acetonitrile were used as mobile phase for gradient elution. After UPLC separation, negative ion mode monitoring was used by electrospray ionization source. The calibration curves showed a good linearity in the range of 1 ng/m L to 50 ng/mL, with the correlation coefficients greater than 0.995. The detection limit was confirmed at 0.05 mg/kg. The matrix recoveries were within 76.90 % to 101.55 %and the relative deviations were lower than 8 %. The method could fully meet the requirements of daily detection and it had the advantages including simple pretreatment, accurate and rapid determination, and high sensitivity. It was suitable for rapid screening and quantitative confirmation of neotame in alcoholic drinks.