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、2.00mg/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。
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 Pro Elut 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.
出处
《湖北农业科学》
北大核心
2014年第19期4698-4700,共3页
Hubei Agricultural Sciences
基金
农业部农药检定所农药登记残留试验项目(2013F421)
