Przybylski Cédric, Segard Christophe
Centre Technique de la Conservation des Produits Agricoles, Laboratoire de Recherche et Développement Analytique, Dury-les-Amiens, France.
J Sep Sci. 2009 Jun;32(11):1858-67. doi: 10.1002/jssc.200900016.
A simple and complete multiresidue method has been developed for the routine determination of 236 pesticides and degradation products, in meat based baby-food. This original approach combines a modified Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method using a triple partitioning extraction step with water/ACN/hexane and a system composed of GC with programmable temperature vaporization injector hyphenated to an IT-MS. Detection was performed in full scan mode, with one quantification ion and one identification ion. We firstly report here the hexane addition in the extraction step to eliminate a major part of lipophile co-extracts. Direct consequences were the increasing of method sensitivity and the diminishment of the frequency of maintenance of the analytical instrument. The recovery data were obtained by spiking blank samples at three concentration levels (10, 50 and 200 microg/kg) over five replicates, yielding average recoveries in the range 70-121% with a RSD evaluated between 2-15%. Linearity was fixed in the range of 10-300 microg/kg with determination coefficients (R2) superior or equal to 0.9814 for all target analytes. Best LODs and LOQs were established as 0.03 and 0.1 microg/kg, respectively. Total instrumental analysis of all molecules was carried out in less than 1 h.
已开发出一种简单且完整的多残留方法,用于常规测定肉类婴儿食品中的236种农药及降解产物。这种原创方法结合了一种改良的快速、简便、廉价、有效、耐用且安全(QuEChERS)的样品制备方法,该方法采用水/乙腈/己烷的三重分配萃取步骤,以及一个由配有程序升温汽化进样器的气相色谱与离子阱质谱联用组成的系统。检测在全扫描模式下进行,使用一个定量离子和一个定性离子。我们在此首次报告在萃取步骤中添加己烷以去除大部分亲脂性共提取物。直接结果是方法灵敏度提高,以及分析仪器维护频率降低。通过在五个重复样中对空白样品进行三个浓度水平(10、50和200微克/千克)的加标来获得回收率数据,平均回收率在70 - 121%范围内,相对标准偏差(RSD)在2 - 15%之间。线性范围设定为10 - 300微克/千克,所有目标分析物的测定系数(R2)均大于或等于0.9814。最低检测限(LOD)和最低定量限(LOQ)分别确定为0.03和0.1微克/千克。所有分子的总仪器分析在不到1小时内完成。