Liu Xingang, Wang Xu, Xu Jun, Dong Fengshou, Song Wencheng, Zheng Yongquan
Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, China.
Biomed Chromatogr. 2011 Oct;25(10):1081-90. doi: 10.1002/bmc.1575. Epub 2011 Mar 4.
A new analytical method using QuEChERS procedure by gas chromatography with a nitrogen-phosphorus detector (GC-NPD) and ion trap mass spectrometry (GC-IT-MS) for the quantitative determination of tebuconazole, trifloxystrobin and its metabolite trifloxystrobin acid has been developed and validated. The analytes were extracted from five fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to GC analysis. The present methods provided sufficient sensitivity as reflected by the values of limit of detection (LOD) and limit of quantification (LOQ) of 0.4-7 and 1.2-20 µg/kg for GC-IT-MS/MS and GC-NPD. The recoveries were, on average, 68-117 and 68-121%, respectively, for three compounds by GC-NPD and GC-IT-MS/MS with intra-day precision achieved with an RSD of 2.7-19.1%. The inter-day precision was better than 15.1% as determined by GC-NPD. The QuEChERS procedure, by using two sorbents (PSA and C18) and the matrix-matched standards, gave satisfactory recoveries and RSD values in different matrices. IT-MS acquisition provided higher specificity and selectivity for pesticides and better limit of detection and quantification. However, the repeatability and precision of NPD method were better compared with IT-MS.
已开发并验证了一种采用QuEChERS方法,结合带有氮磷检测器(GC-NPD)的气相色谱法和离子阱质谱法(GC-IT-MS)对戊唑醇、肟菌酯及其代谢产物肟菌酯酸进行定量测定的新分析方法。使用乙腈从五种水果和蔬菜基质中提取分析物,随后在进行气相色谱分析之前,使用伯仲胺(PSA)或十八烷基硅烷(C18)作为吸附剂进行净化。本方法具有足够的灵敏度,气相色谱-离子阱串联质谱法(GC-IT-MS/MS)和气谱-氮磷检测法(GC-NPD)的检测限(LOD)和定量限(LOQ)值分别为0.4 - 7和1.2 - 20 μg/kg。通过GC-NPD和GC-IT-MS/MS对三种化合物的回收率平均分别为68 - 117%和68 - 121%,日内精密度的相对标准偏差(RSD)为2.7 - 19.1%。气相色谱-氮磷检测法测定的日间精密度优于15.1%。通过使用两种吸附剂(PSA和C18)以及基质匹配标准品的QuEChERS方法,在不同基质中获得了令人满意的回收率和RSD值。离子阱质谱采集对农药具有更高的特异性和选择性,以及更好的检测限和定量限。然而,与离子阱质谱相比,氮磷检测法的重复性和精密度更好。