Wang Kun, Chen Guan-hua, Wu Xian, Shi Jie, Guo Dong-shan
College of Food and Bioengineering, Jiangsu University, Zhenjiang 212013, China.
J Chromatogr Sci. 2014 Feb;52(2):157-63. doi: 10.1093/chromsci/bmt001. Epub 2013 Feb 6.
A new assay of micellar electrokinetic capillary chromatography with sweeping was developed to determine azoxystrobin, kresoxim-methyl and pyraclostrobin in fruits and vegetables. The key factors affecting resolution and peak height were studied and the optimum conditions were obtained for separation and enrichment. The running buffer consisted of 40 mM borate, 25 mM sodium dodecyl sulfate and 15% acetonitrile, and its pH was adjusted to 8.4. The sample was injected for 677 nL and the separation voltage was 25 kV. Under the optimum conditions, the enrichment factors of azoxystrobin, kresoxim-methyl and pyraclostrobin were 861, 550 and 403; the linear dynamic ranges were all 0.01-5.0 mg/L; the limits of detection were 0.002, 0.001 and 0.002 mg/kg; the recoveries of spiked samples were 85.1-98.5%, 87.5-97.0% and 89.1-99.1%, respectively. The assay can meet the requirement of maximum residue limits for these three strobilurin fungicides, and has been applied for determining their residues in fruits and vegetables.
建立了一种新的胶束电动毛细管色谱扫集分析法,用于测定水果和蔬菜中的嘧菌酯、醚菌酯和吡唑醚菌酯。研究了影响分离度和峰高的关键因素,获得了分离和富集的最佳条件。运行缓冲液由40 mM硼酸盐、25 mM十二烷基硫酸钠和15%乙腈组成,pH值调至8.4。进样量为677 nL,分离电压为25 kV。在最佳条件下,嘧菌酯、醚菌酯和吡唑醚菌酯的富集因子分别为861、550和403;线性动态范围均为0.01 - 5.0 mg/L;检测限分别为0.002、0.001和0.002 mg/kg;加标样品的回收率分别为85.1 - 98.5%、87.5 - 97.0%和89.1 - 99.1%。该分析法能够满足这三种甲氧基丙烯酸酯类杀菌剂最大残留限量的要求,并已应用于水果和蔬菜中它们残留量的测定。