Dipartimento di Chimica Farmaceutica e Tossicologica, Università degli Studi di Napoli Federico II, Via D. Montesano 49, 80131 Napoli, Italy.
J Chromatogr A. 2011 Mar 4;1218(9):1253-9. doi: 10.1016/j.chroma.2011.01.006. Epub 2011 Jan 15.
This study proposes a fast, simple and sensitive liquid chromatography diode array detector (LC/UV-DAD)-based method for the simultaneous determination of eight sulfonylurea herbicides (bensulfuron methyl, chlorsulfuron, metsulfuron methyl, primisulfuron methyl, rimsulfuron, thifensulfuron methyl, triasulfuron and tribenuron methyl) in bovine whole milk at concentrations lower than the default limit of 0.01 mg kg(-1) allowed by current legislation (Regulation EC/396/2005 and following Annexes). An effective one-step solid phase extraction (SPE) and clean up procedure was defined with use of Chem Elut cartridges, providing good recoveries for all the analytes tested and with no matrix effects affecting method accuracy. Separation of herbicides was obtained on a C(18) column by acetonitrile- water gradient elution. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(α)) and detection capability (CC(β)). Typical recoveries ranged between 78.4% and 99.7%, at the maximum residue limits (MRLs) levels established by Regulation EC/396/2005, with relative standard deviations (RSD) no larger than 10%.
本研究提出了一种快速、简单和灵敏的基于液相色谱二极管阵列检测器（LC/UV-DAD）的方法，用于同时测定牛奶中八种磺酰脲类除草剂（苄嘧磺隆、氯磺隆、甲磺胺隆、醚苯磺隆、吡嘧磺隆、噻吩磺隆、三氟啶磺隆和三甲苯隆）的浓度，低于现行法规（EC/396/2005 号法规及后续附件）规定的默认限量 0.01mg/kg。采用 Chem Elut 萃取柱进行了有效的一步固相萃取（SPE）和净化程序，为所有测试的分析物提供了良好的回收率，且无基质效应影响方法准确性。在 C(18)柱上，通过乙腈-水梯度洗脱实现了除草剂的分离。方法验证符合欧洲委员会 2002/657/EC 决定的标准，包括线性、回收率、精密度、特异性、决策限（CC(α))和检测能力（CC(β))。在 EC/396/2005 法规规定的最大残留限量（MRLs）水平下，典型回收率在 78.4%至 99.7%之间，相对标准偏差（RSD）不超过 10%。
