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中国精品科技期刊2020
林正锋,李实飞,黄杰英,等. 液相色谱-串联质谱法测定乳制品中四种常用香料[J]. 食品工业科技,2021,42(21):271−278. doi: 10.13386/j.issn1002-0306.2021010170.
引用本文: 林正锋,李实飞,黄杰英,等. 液相色谱-串联质谱法测定乳制品中四种常用香料[J]. 食品工业科技,2021,42(21):271−278. doi: 10.13386/j.issn1002-0306.2021010170.
LIN Zhengfeng, LI Shifei, HUANG Jieying, et al. Determination of 4 Kinds of Frequently-used Spices in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(21): 271−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010170.
Citation: LIN Zhengfeng, LI Shifei, HUANG Jieying, et al. Determination of 4 Kinds of Frequently-used Spices in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(21): 271−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010170.

液相色谱-串联质谱法测定乳制品中四种常用香料

Determination of 4 Kinds of Frequently-used Spices in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了液相色谱-串联质谱法测定乳制品中麦芽酚、乙基麦芽酚、香兰素和乙基香兰素四种香料的方法。样品经水-叔丁基甲醚(MTBE)提取后,采用0.2 mol/L氢氧化钠溶液萃取醚相中的香料(碱醚体积比为1:5)来实现净化并使之富集到水相。选用HSS T3色谱柱进行液相分离,甲醇-0.05%甲酸作为流动相进行梯度洗脱,质谱分析采用电喷雾正离子电离,多反应监测模式。该方法在2.0~100.0 ng/mL浓度范围内线性关系良好,决定系数R2>0.995,定量限可达8.0 μg/kg,四种香料化合物在8种乳制品中基质效应在80%~100%之间,为弱基质抑制效应,实际检测中可不考虑基质效应。不同乳制品在10、25和100 μg /kg三个加标水平下,平均回收率为67.7%~104.8%,相对标准偏差为2.5%~11.9% (n=6)。该法具有操作简便、灵敏度高、准确可靠的优点,适用于乳制品中四种香料的检测。

     

    Abstract: An analytical method based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for detecting 4 kinds of frequently-used spices (maltol, ethyl-maltol, vanillin and ethyl-vanillin) in dairy products. The samples were extracted by water and tert butyl methyl ether, the supernatants were extracted by 0.2 mol/L sodium hydroxide solution alkali solution (the volume ratio of alkali solution to MTBE was 1:5) for purification and enrichment of target composes to the aqueous phase. The separation of these 4 compounds was carried out by a HSS T3 column and the mobile phase performed on 0.05% formic acid aqueous solution-methanol by gradient elution, electrospray ionization source (ESI) was applied and operated in the positive mode. Multiple reaction monitoring (MRM) mode was used to monitor ions. The results showed that the method had a good linearity range between 2.0~100.0 ng/mL (R2>0.995) and the detection limits were as low as 8.0 μg/kg. The matrix effects of 4 kinds of spices in different dairy products showed week matrix suppression effects and ranged from 80%~100%, suggesting the matrix effects advisably being ignored in routine testing. The average recoveries of the targeted compounds range from 67.7% to 104.8% at spiked levels of 10, 25 and 100 μg /kg, and relative standard deviations range from 2.5% to 11.9% (n=6). The method is simple, sensitive, accurate and reliable.

     

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