液相色谱―质谱法对柑橘中吡唑醚菌酯残留的检测.docVIP

液相色谱―质谱法对柑橘中吡唑醚菌酯残留的检测 摘要：建立了高效液相色谱-质谱法检测柑橘中吡唑醚菌酯残留量的方法。柑橘经乙腈提取，Carbon/NH2柱净化，实现样品的制备。在岛津VP-ODS色谱柱上，以乙腈和0.1%甲酸溶液（70+30，V/V）为流动相，采用电喷雾正离子（ESI+） SIM扫描模式，以m/z 388为定量检测离子，吡唑醚菌酯保留时间为6.3 min，在0.01～0.50 mg/L内呈良好的线性关系， R2为0.999 8。在柑橘样品（全果、果肉）中添加0.05、 0.20、 2.00 mg/kg的吡唑醚菌酯标准样品，其回收率为101%～115%，相对标准偏差（RSD）均小于5%。最低检出量（S/N 10）为3.4×10-13 g。准确度和精密度均能满足检测要求。 关键词：吡唑醚菌酯；残留；液相色谱-质谱 中图分类号：O657.63 文献标识码：A 文章编号：0439-8114（2014）19-4698-03 DOI：10.14088/j.cnki.issn0439-8114.2014.19.050 Determination of Pyraclostrobin Residue in Citrus by LC-MS LIU Jun， ZHANG Xian， SHEN Jing， QI Zhi-hong （Agricultural Quality Standards and Inspection Technology Research Institute， Hubei Academy of Agricultural Science， Wuhan 430064，China） Abstract： A method for determing pyraclostrobin residues in whole fruit of citrus and citrus pulp was established with by LC-ESI-MS. Pyraclostrobin residues were extracted from samples with acetonitrile， cleaned up by ProElut Carbon/NH2 SPE to achieve sample preparation， and separated on the Shimadzu VP-ODS column， using a mixture of acetonitrile and 0.1% formic acid solution （70+30，V/V） as mobile phase. Determination was made by using ESI under the mode of SIM. Quantitative detection of ions was m/z 388， the retention time of pyraclostrobin was 6.3 min. Linearity were held in the ranges of 0.01～0.50 mg/L with the correlation coefficient of 0.999 8. The average recoveries of pyraclostrobin in whole fruit of citrus and citrus pulp at the spiked amounts of 0.05～2.00 mg/kg were 101%～115%， and the relative standard deviation was lower than 5.0%. The limit of detectable amount （S/N 10） was 1.3×10-13 g. The accuracy and precision of this method can meet the requirements of detection. Key words： pyraclostrobin； residue； LC-ESI-MS 吡唑醚菌酯（Pyraclostrobin），又名唑菌胺酯、百克敏，是兼具吡唑结构的甲氧基丙烯酸酯类杀菌剂，是由德国巴斯夫公司于1993年开发，2001年登记并上市，目前已用于100多种作物上，可以防治由多种真菌病原引起的病害[1]，同样能够防治柑橘的酸腐病、青霉病。目前，关于吡唑醚菌酯的检测方法有吴洁珊等[2]采用气相色谱测定柑橘中多种甲氧基丙烯酸酯类杀菌剂的残留量；薄海波等[3]采用气相色谱―质谱法测定食品中甲氧基丙烯酸酯类杀菌剂残留；徐英江等[4]采用液相色谱串联质谱测定蔬菜中残留的唑菌胺酯；以及在西瓜