Zhou Yao, Yang Huiqin, Shi Yiyin, Chen Jiaxian, Zhu Jian, Deng Xiaojun, Guo Dehua
Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.
Se Pu. 2017 Sep 8;35(9):970-979. doi: 10.3724/SP.J.1123.2017.05009.
A method was developed for the simultaneous determination of six strobilurin fungicide (-metominostrobin, azoxystrobin, kresoxim-methyl, picoxystrobin, pyraclostrobin and trifloxystrobin) residues in orange, banana, apple and pineapple samples by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The fragmentation routes of all the compounds were explained by the aid of a fragment predicting software ACD Lab/MS Fragmenter. The samples were extracted by acetonitrile, then cleaned up by amino solid phase extraction cartridges (SupelClean LC-NH). The extracts were separated on a ACQUITY UPLC BEH C column (50 mm×2.1 mm, 1.7 μm) with gradient elution. Acetonitrile containing 0.1% (v/v) formic acid and 10 mmol/L ammonium acetate containing 0.1% (v/v) formic acid were used as mobile phases. The samples were detected by electrospray ionization (ESI)-MS/MS in positive ion and multiple reaction monitoring (MRM) mode, quantified by external standard method. Good linearities were obtained in the range of 5-100 μg/L (for pyraclostrobin, 1-20 μg/L) with correlation coefficients () greater than 0.999. The recoveries ranged from 60.4% to 120% with the relative standard deviations between 2.15% and 15.1% (=6). The developed method can meet the inspection of the six strobilurin residues in the orange, banana, apple and pineapple samples.
建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定橙子、香蕉、苹果和菠萝样品中6种甲氧基丙烯酸酯类杀菌剂(甲氨基阿维菌素苯甲酸盐、嘧菌酯、醚菌酯、啶氧菌酯、吡唑醚菌酯和肟菌酯)残留量的方法。借助碎片预测软件ACD Lab/MS Fragmenter对所有化合物的裂解途径进行了解释。样品用乙腈提取,然后用氨基固相萃取柱(SupelClean LC-NH)净化。提取物在ACQUITY UPLC BEH C柱(50 mm×2.1 mm,1.7 μm)上进行梯度洗脱分离。以含0.1%(v/v)甲酸的乙腈和含0.1%(v/v)甲酸的10 mmol/L醋酸铵为流动相。样品采用电喷雾电离(ESI)-MS/MS在正离子和多反应监测(MRM)模式下进行检测,外标法定量。在5-100 μg/L范围内(吡唑醚菌酯为1-20 μg/L)获得了良好的线性关系,相关系数()大于0.999。回收率在60.4%至120%之间,相对标准偏差在2.15%至15.1%之间(n=6)。所建立的方法能够满足橙子、香蕉、苹果和菠萝样品中6种甲氧基丙烯酸酯类残留量的检测要求。