Hu Dan, Xu Xu, Cai Tian, Wang Wei-Ying, Wu Chun-Jie, Ye Li-Ming
1 West China School of Pharmacy, Sichuan University, Chengdu 610041, People's Republic of China.
2 Chengdu Institute of Organic Chemistry, University of Chinese Academy of Sciences, Chengdu 610041, People's Republic of China; and.
J Food Prot. 2017 Dec;80(12):2112-2118. doi: 10.4315/0362-028X.JFP-17-228.
A rapid and sensitive analytical method based on high-performance liquid chromatography-tandem mass spectrometry was developed and validated for the determination of isopyrazam (IZM) and azoxystrobin (AZT) in cucumbers. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used as the pretreatment procedure. The samples were extracted with acetonitrile and cleaned up with octadecylsilyl silica (C18) and graphite carbon black. The proposed method resulted in satisfactory recovery of IZM and AZT (91.48 to 114.62%), and relative standard deviations were less than 13.1% at fortification concentrations of 1, 20, and 500 μg kg (n = 3). The limits of quantification for IZM and AZT were 0.498 and 0.499 μg kg, respectively, which are far below the maximum residue level (0.5 mg kg) established for this type of sample. Matrix effects were also evaluated. This study established a sensitive and fast method for the detection of IZM and AZT in cucumber samples.
建立了一种基于高效液相色谱-串联质谱的快速灵敏分析方法,并对其进行了验证,用于测定黄瓜中的异菌脲(IZM)和嘧菌酯(AZT)。采用改进的QuEChERS(快速、简便、廉价、有效、耐用和安全)方法作为预处理程序。样品用乙腈提取,并用十八烷基硅烷键合硅胶(C18)和石墨化炭黑净化。该方法对IZM和AZT的回收率令人满意(91.48%至114.62%),在1、20和500 μg/kg的加标浓度下(n = 3),相对标准偏差小于13.1%。IZM和AZT的定量限分别为0.498和0.499 μg/kg,远低于针对此类样品设定的最大残留限量(0.5 mg/kg)。还评估了基质效应。本研究建立了一种灵敏快速的方法用于检测黄瓜样品中的IZM和AZT。