Shen Weijian, Gui Qianwen, Yu Keyao, Sun Ningning, Zhao Zengyun, Shen Chongyu, Wu Bin, Jiang Yuan, Chu Xiaogang
Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China.
Se Pu. 2009 Jan;27(1):91-5.
A confirmatory method is proposed for the determination of 12 azole fungicide residues in beans and corn with the technique of offline disperse solid phase extraction (DSPE) and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The pesticides interested were extracted from the samples with acetonitrile containing 1% acetic acid and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate plus sodium acetate followed by a simple cleanup step known as dispersive solid-phase extraction. The aliquot was determined and confirmed by GC-NCI/MS using external standard method. The recoveries of all pesticides were between 70% and 130% at the three spiked levels, 10 microg/kg, 20 microg/kg and 40 microg/kg. The relative standard deviations were less than 13.9%. The linearity of method was good from 50 to 1 000 microg/L. The limits of quantification (LOQ) were less than 8 microg/kg. The method is selective with no interference and is suitable for the confirmatory of pesticide residues in beans and corn.
本文提出了一种采用离线分散固相萃取(DSPE)和气相色谱-负化学电离质谱联用(GC-NCI/MS)技术测定豆类和玉米中12种唑类杀菌剂残留量的确证方法。用含1%乙酸的乙腈从样品中提取目标农药,加入无水硫酸镁和乙酸钠进行液液分配,随后进行简单的净化步骤即分散固相萃取。取部分溶液,采用外标法通过GC-NCI/MS进行测定和确证。在10μg/kg、20μg/kg和40μg/kg三个加标水平下,所有农药的回收率在70%~130%之间,相对标准偏差小于13.9%。该方法在50~1000μg/L范围内线性良好,定量限小于8μg/kg。该方法选择性好,无干扰,适用于豆类和玉米中农药残留的确证分析。