Streamlined sample preparation procedure for determination of perchlorate anion in foods by ion chromatography-tandem mass spectrometry
Streamlined sample preparation procedure for determination of perchlorate anion in foods by ion chromatography-tandem mass spectrometry
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DOI：
10.1016/j.aca.2006.01.005
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发表时间：
2006-05-10
影响因子：
6.2
通讯作者：
Hopper, ML
中科院分区：
文献类型：
--
作者：
Krynitsky, AJ;Niemann, RA;Hopper, ML
建立了一种快速、灵敏、特异的食品中高氯酸根含量的测定方法。这些食品包括高水分水果和蔬菜、低水分食品(如面粉和玉米粉)和婴儿食品。对现有的样品制备程序进行了改进，将样品测试部分从100克减少到5克或10克，提取溶剂从150克减少到20-40毫升，并将混合萃取-真空过滤和相关的大型玻璃器皿改为在一个小锥形管中进行简单的洗涤-离心法。所有涉及的基质通用程序：萃取、离心法、石墨化碳固相萃取(SPE)净化和离子色谱-串联质谱仪(IC-MS/MS)分析。采用Waters IC-Pak阴离子HR柱(4.6 mm×75 mm)，以100 mm醋酸铵为洗脱剂，乙腈/水为50：50(v/v)流动相，流速为0.35ml/min。采用电喷雾电离(ESI)负离子模式的三级四极质谱计检测高氯酸根离子。用O-18(4)标记的高氯酸盐阴离子内标校正任何基质影响。方法检出限为：水果、蔬菜和婴幼儿食品中1.0微克/千克；干品中3.0微克/千克。强化试验部分的回收率为80%-120%。高氯酸盐阴离子残留量的测定结果与用公开方法分析的可比商品或产品的结果一致。爱思唯尔出版公司(Elsevier B.V.)
A rapid, sensitive, and specific method was developed for the determination of perchlorate anion in foods. The foods included high moisture fruits and vegetables, low moisture foods (e.g. wheat flour and corn meal), and infant foods. Improvements to existing procedures were made in sample preparation that reduced sample test portion size from 100 to 5 or 10 g, extraction solvent volume from 150 to 20-40 nil, and replaced blending extraction-vacuum filtration and their associated large glassware with a simple shakeout-centrifugation in a small conical tube. Procedures common to all matrices involved: extraction, centrifugation, graphitized carbon solid phase extraction (SPE) cleanup, and ion chromatography-tandem mass spectrometry (IC-MS/MS) analysis. A Waters IC-Pak Anion HR column (4.6 mm x 75 mm) was eluted with 100 mM ammonium acetate in 50:50 (v/v) acetonitrile/water mobile phase at a rate of 0.35 ml/min. A triple stage quadrupole mass spectrometer, equipped with electrospray ionization (ESI) in the negative ion mode, was used to detect perchlorate anion. An O-18(4)-labeled perchlorate anion internal standard was used to correct for any matrix effects. The method limit of quantitation (LOQ) was: 1.0 mu g/kg in fruits, vegetables, and infant foods; 3.0 mu g/kg in dry products. Fortified test portions gave 80-120% recoveries. Determination of incurred perchlorate anion residues agreed well with results for comparable commodities or products analyzed by published methods. Published by Elsevier B.V.