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采用液相色谱/质谱联用和气相色谱/质谱联用技术测定并确证食品中的五种酚类抗氧化剂。

Determination and confirmation of five phenolic antioxidants in foods by LC/MS and GC/MS.

作者信息

Tsuji Sumiko, Nakanoi Maki, Terada Hisaya, Tamura Yukio, Tonogai Yasuhide

机构信息

Division of Food Chemistry, Osaka Branch, National Institute of Health Sciences, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2005 Jun;46(3):63-71. doi: 10.3358/shokueishi.46.63.

DOI:10.3358/shokueishi.46.63
PMID:16042291
Abstract

Identification and determination of butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), nordihydroguaiaretic acid (NDGA), propyl gallate (PG) and tert-butylhydroquinone (TBHQ) by means of LC/MS and GC/MS were examined. These five phenolic antioxidants were detected as their pseudo-molecular ions [M-H]- by LC/MS using a Shim-pack FC-ODS column with drying gas. Moreover, BHA, BHT and TBHQ were detected based on their mass fragment ions by GC/MS. Decomposition of TBHQ, NDGA and PG during analysis could be prevented by the addition of L-ascorbic acid (AsA) to the extraction solvent. All five antioxidants were extracted from nikuman, olive oils, peanut butter, pasta sauce and chewing gum with a mixture of acetonitrile-2-propanol-ethanol (2:1:1) containing 0.1% AsA (AsA mixture), which had been cooled in a freezer and filtered. One part filtrate and 5 parts water were mixed and placed on a Mega-Bond Elut C18 cartridge, except in the case of chewing gum. Lipids in foods were removed on a C18 cartridge by washing with 5 mL of 5% acetic acid, and antioxidants were eluted with 5 mL of AsA mixture. The antioxidants spiked into nikuman, olive oil, peanut butter, pasta sauce and chewing gum were successfully identified and their concentrations determined by LC/MS, and GC/MS with good recoveries.

摘要

通过液相色谱-质谱联用(LC/MS)和气相色谱-质谱联用(GC/MS)对丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)、去甲二氢愈创木酸(NDGA)、没食子酸丙酯(PG)和叔丁基对苯二酚(TBHQ)进行了鉴定和测定。使用配备干燥气体的Shim-pack FC-ODS柱,通过LC/MS将这五种酚类抗氧化剂检测为它们的准分子离子[M-H]-。此外,通过GC/MS根据BHA、BHT和TBHQ的质量碎片离子进行检测。在萃取溶剂中添加L-抗坏血酸(AsA)可防止分析过程中TBHQ、NDGA和PG的分解。使用含有0.1% AsA(AsA混合物)的乙腈-2-丙醇-乙醇(2:1:1)混合物从肉包、橄榄油、花生酱、意大利面酱和口香糖中萃取所有五种抗氧化剂,该混合物已在冰箱中冷却并过滤。除口香糖外,将一份滤液与五份水混合,置于Mega-Bond Elut C18柱上。通过用5 mL 5%乙酸洗涤,在C18柱上去除食品中的脂质,并用5 mL AsA混合物洗脱抗氧化剂。通过LC/MS和GC/MS成功鉴定了添加到肉包、橄榄油、花生酱、意大利面酱和口香糖中的抗氧化剂,并测定了它们的浓度,回收率良好。

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