色谱2018，Vol.36Issue(1)：17-22,6.DOI:10.3724/SP.J.1123.2017.09034
高效液相色谱-串联质谱法测定荔枝花粉和花蜜中腈菌唑和苯醚甲环唑残留
Determination of myclobutanil and difenoconazole residues in pollen and honey of litchi by high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
An effective method was developed for the determination of two major fungicides including myclobutanil and difenoconazole residues in pollen and honey of litchi by modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The pollen and honey samples were all extracted by acetonitrile,the pollen samples were cleaned-up by 0.9 g anhydrous magnesium sulfate(MgSO4),0.15 g primary secondary amine (PSA)and 0.15 g C18;the honey samples were cleaned-up by 0.9 g MgSO4and 0.15 g PSA. The 0.1%(v/v)formic acid aqueous solution-acetonitrile(25 :75,v/v)were used as the mobile phases. The extracts were separated on a Poroshell-120 EC-C18chromatographic column,the positive electrospray ion(ESI+)source and selected ion monitoring(SIM)mode were used. The analytes were quantified by the matrix matching standard solutions. The matrix matched standard solutions of myclobutanil and difenoconazole showed good linearities in the range of 1-100 μg/L,and the correlation coefficients(r2)were all above 0.999 0. The limits of detection(LODs)of myclobutanil and difenoconazole were 0.25 μg/kg and 0.50 μg/kg, respectively. The limits of quantification(LOQs)of myclobutanil and difenoconazole were 0.83 μg/kg and 1.7 μg/kg,respectively. The average recoveries of myclobutanil and difenoconazole in pollen and honey samples were 87.0%-95.2% and 90.1%-96.4% with the relative standard deviations of 1.2%-3.6% and 0.7%-4.1%,respectively. The method is quick,easy and sensi-tive,and it is suitable for the rapid determination and trace analysis of myclobutanil and difeno-conazole in pollens and honeys of litchi. The method can provide data support for the exposure risk assessment of bees and other pollination insects.关键词
高效液相色谱-串联质谱/QuEChERS/腈菌唑/苯醚甲环唑/荔枝花粉和花蜜Key words
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/QuEChERS/myclobutanil/difenoconazole/pollen and honey of litchi分类
化学化工引用本文复制引用
王思威,刘艳萍,孙海滨,杜兰娟,徐能莉..高效液相色谱-串联质谱法测定荔枝花粉和花蜜中腈菌唑和苯醚甲环唑残留[J].色谱,2018,36(1):17-22,6.基金项目
国家荔枝龙眼产业技术体系(CARS-33-16) （CARS-33-16）
广东省农业科学院院长基金(201707). Foundation item:China Litchi and Longan Research System(No. CARS-33-16) （201707）
President Fund of Guangdong Academy of Agricultural Sciences(No. 201707). （No. 201707）
