Lee Jeong-Min, Park Jin-Won, Jang Gi-Chul, Hwang Keon-Joong
KT&G Central Research Institute, 302 Shinseong-dong, Yuseong-gu, Daejeon 305-805, Republic of Korea.
J Chromatogr A. 2008 Apr 11;1187(1-2):25-33. doi: 10.1016/j.chroma.2008.02.035. Epub 2008 Feb 14.
This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). We compared with the three-sample preparation methods of pesticide residues in tobacco such as the conventional liquid-liquid extraction (LLE), pressurized liquid extraction (PLE) and QuEChERS (quick, easy, cheap, effective, rugged and safe) methods. These methods were validated for 49 pesticides in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. LLE with acetonitrile, and PLE with acetone were followed by solid-phase extraction (SPE) and analyzed by GC-MS/MS. In QuEChERS method, the effects of sorbents, such as primary secondary amine (PSA), octadecylsilane (C(18)) and graphitized carbon black (GCB), and matrix of the analytes in tobacco types, such as flue-cured, burley and oriental were investigated. MS/MS acquisition provided high specificity and selectivity for pesticides and low limit of detection and quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. The method yielded higher and more consistent recoveries of these analytes than LLE and PLE. QuEChERS method was no needed to be complex clean-up procedure and would be used to rapid and sensitive analysis of pesticides as an alternative to LLE and PLE methods.
本研究旨在应用更快速准确的样品制备方法,以及气相色谱-三重四极杆质谱联用仪(GC-MS/MS)对分析物检测的高选择性和高灵敏度。我们比较了烟草中农药残留的三种样品制备方法,如传统的液液萃取(LLE)、加压液体萃取(PLE)和QuEChERS(快速、简便、廉价、高效、耐用且安全)方法。这些方法在CORESTA农药咨询委员会指南中针对49种农药进行了验证,适用于GC-MS/MS测定。乙腈液液萃取法和丙酮加压液体萃取法之后进行固相萃取(SPE),并通过GC-MS/MS进行分析。在QuEChERS方法中,研究了吸附剂如伯仲胺(PSA)、十八烷基硅烷(C(18))和石墨化炭黑(GCB)的影响,以及烤烟、白肋烟和香料烟等烟草类型中分析物的基质影响。串联质谱采集为农药提供了高特异性和选择性,以及低检测限和定量限。仅使用PSA的QuEChERS方法和基质匹配标准品在三种烟草中给出了良好的回收率和相对标准偏差值。该方法对这些分析物的回收率高于液液萃取法和加压液体萃取法,且更具一致性。QuEChERS方法无需复杂的净化程序,可作为液液萃取法和加压液体萃取法的替代方法,用于农药的快速灵敏分析。