Analysis of coffee for the presence of acrylamide by LC-MS/MS

Analysis of coffee for the presence of acrylamide by LC-MS/MS
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DOI:
10.1021/jf0349634
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发表时间:
2004-04-07
影响因子:
6.1
通讯作者:
Musser, SM
Musser, SM
中科院分区:
农林科学1区
文献类型:
--
作者:
Andrzejewski, D;Roach, JAG;Musser, SM

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各种流行的速溶咖啡,地面,和酿造咖啡进行了分析,使用改进的液相色谱-串联质谱(LC-MS/MS)方法,专门开发用于测定食品中的丙烯酰胺。在提取和净化之前,用C-13(3)标记的丙烯酰胺作为内标物掺入咖啡测试部分。研磨咖啡(1 g)和速溶咖啡(0.5 g)通过与9 mL水振荡20 min进行提取。将冲泡咖啡测试部分(9 mL)通过净化程序进行提取,无需进一步用提取溶剂稀释。通过使1.5mL首先通过Oasis HLB(亲水/亲脂共聚物吸附剂)固相萃取(SPE)柱,然后通过Bond Elut-Accucat(阳离子和阴离子交换吸附剂)SPE柱来净化咖啡测试部分。通过阳离子电喷雾LC-MS/MS分析净化的浸提液。MS/MS数据用于检测、确认和定量丙烯酰胺。该方法的定量限为10 ng/g的地面和速溶咖啡和1.0 ng/mL的煮咖啡。未煮咖啡渣中丙烯酰胺的含量范围为45至374纳克/克,速溶咖啡晶体中为172至539纳克/克,煮咖啡中为6至16纳克/毫升。
A variety of popular instant, ground, and brewed coffees were analyzed using a modified liquid chromatography-tandem mass spectrometry (LC-MS/MS) method specifically developed for the determination of acrylamide in foods. Coffee test portions were spiked with C-13(3)-labeled acrylamide as an internal standard prior to their extraction and cleanup. Ground coffees (1 g) and instant coffees (0.5 g) were extracted by shaking with 9 mL of water for 20 min. Brewed coffee test portions (9 mL) were taken through the cleanup procedure without further dilution with extraction solvent. Coffee test portions were cleaned up by passing 1.5 mL first through an Oasis HLB (hydrophilic/lipophilic copolymer sorbent) solid phase extraction (SPE) cartridge and then a Bond Elut-Accucat (cation and anion exchange sorbent) SPE cartridge. The cleaned up extracts were analyzed by positive ion electrospray LC-MS/MS. The MS/MS data was used to detect, confirm, and quantitate acrylamide. The limit of quantitation of the method was 10 ng/g for ground and instant coffees and 1.0 ng/mL for brewed coffee. The levels of acrylamide ranged from 45 to 374 ng/g in unbrewed coffee grounds, from 172 to 539 ng/g in instant coffee crystals, and from 6 to 16 ng/mL in brewed coffee.