Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok 10330, Thailand.
Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok 10330, Thailand.
Food Chem. 2014 Jun 15;153:44-51. doi: 10.1016/j.foodchem.2013.12.029. Epub 2013 Dec 12.
A simple and efficient QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation method was modified to provide good analytical results for 14 mycotoxins in rice. The method involved mixing sample with acidified aqueous acetonitrile, followed by salt-out liquid partitioning using MgSO4, NaCl, and citrate buffer salts. The extract was cleaned-up by dispersive solid-phase extraction with MgSO4, PSA, C18, and alumina-neutral. The analysis was performed using ultra-high performance liquid chromatography coupled to triple-quadrupole tandem mass spectrometry (UHPLC-MS/MS). Throughout the validation experiments, 70-98% overall recoveries were achieved with RSDs ⩽ 7% for most analytes at concentrations 10-100 μg kg(-1). Limit of detections were 0.5-15 μg kg(-1). Inter-laboratory precision was performed by proficiency testing, |z|⩽ 2 was considered satisfactory. We compared our modified QuEChERS method against sample preparation using an immunoaffinity column; the recovery and specificity were comparable for the two methods, but the QuEChERS approach was more time- and cost-effective.
一种简单高效的 QuEChERS(快速、简单、廉价、有效、耐用、安全)样品制备方法经过修改,可用于大米中 14 种霉菌毒素的良好分析结果。该方法涉及将样品与酸化的乙腈水溶液混合,然后使用硫酸镁、氯化钠和柠檬酸盐缓冲盐进行盐析液分配。用硫酸镁、PSA、C18 和中性氧化铝进行分散固相萃取对提取物进行净化。使用超高效液相色谱-串联三重四极杆质谱(UHPLC-MS/MS)进行分析。在整个验证实验中,对于大多数浓度为 10-100μgkg-1 的分析物,总回收率为 70-98%,相对标准偏差(RSD)⩽7%。检测限为 0.5-15μgkg-1。通过能力验证进行实验室间精密度评估,|z|⩽2 被认为是令人满意的。我们将改良的 QuEChERS 方法与免疫亲和柱的样品制备方法进行了比较;两种方法的回收率和特异性相当,但 QuEChERS 方法更省时、更经济。