National Agricultural Products Quality Management Service, Products Safety Inspection Laboratory, Gwangsan-gu, Gwangju, South Korea.
J Chromatogr A. 2011 Jul 15;1218(28):4366-77. doi: 10.1016/j.chroma.2011.05.021. Epub 2011 May 14.
This study describes a new QuEChERS method referred to as the dry ice-partitioning QuEChERS method. This current method can be differentiated from the other QuEChERS methods in the sense that it uses dry ice rather than salts or buffers to extract and partition pesticides in the first extraction step. The dry ice-partitioning QuEChERS method consists of extraction method A (for detection of the acetonitrile layer) and extraction method B (for detection of both acetonitrile and aqueous layers). The extraction efficiency was then compared with the citrate-buffering QuEChERS method by means of recovery. Recovery values of the tested 168 pesticides were above 76%, with relative standard deviations of less than 20%. Certain problematic pesticides, including benfuracarb, carbosulfan, dichlofluanid, probenazole, pymetrozine, tolylfluanid, TFNA, and TFNG evidenced acceptable recoveries via the dry ice-partitioning QuEChERS method compared to the less than 70% recoveries of the citrate-buffering QuEChERS method examined herein. The matrix effect of paprika on the method developed herein was not significant, and matrix-matched calibration was performed well, with an r(2)≥0.99. The dry ice-partitioning QuEChERS method is capable of detecting the aqueous layer as well as the acetonitrile layer; this interesting feature makes it worth in application as an alternative QuEChERS method for the multiresidue analysis of pesticides within a broad polarity range in various matrices.
本研究描述了一种新的 QuEChERS 方法,称为干冰分配 QuEChERS 方法。与其他 QuEChERS 方法相比,该方法的不同之处在于它在第一步提取中使用干冰而不是盐或缓冲液来提取和分配农药。干冰分配 QuEChERS 方法由提取方法 A(用于检测乙腈层)和提取方法 B(用于检测乙腈和水层)组成。然后通过回收率比较了提取效率与柠檬酸缓冲 QuEChERS 方法。在所测试的 168 种农药中,回收率均高于 76%,相对标准偏差小于 20%。某些有问题的农药,包括苯丁锡、克百威、双氯氟脲、丙环唑、吡虫啉、甲苯氟脲、TFNA 和 TFNG,通过干冰分配 QuEChERS 方法的回收率可接受,而本文研究的柠檬酸缓冲 QuEChERS 方法的回收率低于 70%。辣椒粉对本文所开发方法的基质效应不显著,基质匹配校准效果良好,r(2)≥0.99。干冰分配 QuEChERS 方法能够检测水层和乙腈层;这个有趣的特点使其值得作为一种替代 QuEChERS 方法,用于各种基质中广泛极性范围内的农药多残留分析。