超高效液相色谱-串联质谱法测定蛋白胨中6种脂溶性维生素  

Determination of 6 kinds of fat-soluble vitamins in peptone using ultra performance liquid chromatography-tandem mass spectrometry

作　　者：莫日根 辛慧 张晓东 杜艳 朱叶青 MO Ri-Gen;XIN Hui;ZHANG Xiao-Dong;DU Yan;ZHU Ye-Qing(Hohhot Food Inspection Institute,Hohhot 010090,China;Inner Mongolia Autonomous Region Institute of Drug Inspection,Hohhot 010010,China)

机构地区：[1]呼和浩特市食品检验所,呼和浩特010090 [2]内蒙古自治区药品检验研究院,呼和浩特010010

出　　处：《食品安全质量检测学报》2020年第20期7436-7441,共6页Journal of Food Safety and Quality

基　　金：科技部重点专项(2017YFC1601400)。

摘　　要：目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定蛋白胨中6种脂溶性维生素的分析方法。方法样品经甲醇-正己烷(8:2,V/V)混合溶液提取,Syncronis C18色谱柱(100 mm×2.1 mm,1.7μm)分离,以0.1%(V/V)甲酸甲醇溶液(含10mmol/L甲酸铵)为流动相进行洗脱,流速为0.2 mL/min。采用电喷雾电离源、正离子扫描、多反应监测模式(multiple reaction monitoring,MRM)进行检测。结果6种脂溶性维生素在各自质量浓度范围内相关系数(r2)均大于0.999,线性关系良好,检出限为0.026~1.109 mg/kg,定量限为0.085~3.696 mg/kg,相对标准偏差均<3%(n=6),且在不同添加水平下的回收率为81.5%~114.8%。结论该方法操作简单,重现性好,准确度高,适用于蛋白胨中6种脂溶性维生素的测定。Objective To establish a method for the simultaneous determination of 6 kinds of fat-soluble vitamins in peptone using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The samples were extracted by methanol hexane(8:2, V:V) solution, separated by Syncronis C18 column(100 mm×2.1 mm, 1.7 μm), eluted with 0.1%(V:V) formic acid methanol solution(containing 10 mmol/L ammonium formate) as mobile phase, and the flow rate was 0.2 mL/min. Positive electrospray ionization(ESI+) and multiple reaction monitoring mode were used for detection. Results The correlation coefficients(r2) of the 6 fat-soluble vitamins in their linear ranges were greater than 0.999. The limits of detection were in the range of 0.026-1.109 mg/kg, and the limits of quantitation were 0.085-3.696 mg/kg. The relative standard deviations of the method were less than 3%(n=6), and the average recoveries were 81.5%-114.8% at different spiked levels. Conclusion This method is simple, sensitive and accurate, which is suitable for the determination of 6 fat-soluble vitamins in peptone.

关 键 词：脂溶性维生素 蛋白胨 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TQ421.22[理学—化学]