固相萃取-气相色谱-质谱联用法测定食品中丙环唑残留量

GC-MS Determination of Residual Amount of Propiconazole in Foodstuffs with Separation by Solid Phase Extraction

提出了18种食品基质中丙环唑残留量的气相色谱-质谱联用分析方法。样品中丙环唑利用乙腈或乙酸乙酯提取,C18和活性炭串联固相萃取柱净化,采用DB-1701弹性毛细管色谱柱进行分离。采用气相色谱-质谱电子轰击电离源和选择离子监测模式进行测定。在0.02～5.0mg.L-1范围内丙环唑标准溶液的峰面积与浓度呈线性关系(r=0.9995),在0.01,0.02,0.05mg.kg-13个添加水平下丙环唑的回收率在70%～115%之间,相对标准偏差(n=6)小于10.2%,检出限(3S/N)为0.004mg·kg-1。

Residual amounts of propiconazole, a bactericide, in foodstuffs of 18 different kinds of matrixes were determined by GC and MS in hyphenation. The sample was extracted with acetonitrile or ethyl acetate according to its variety, and the propiconazole in the extract was purified by passing through C18 SPE column and active carbon column in succession. In the GC-MS analysis, DB-1701 capillary chromatographic column was used for separation, and modes of electron bombardment ionization ion source （EI） and selective ion monitoring （SIM） were adopted for measurement. Linear relationship between values of peak area and mass concentration of propieonazole was kept in the range of 0. 02-5. 0 mg · L^-1, and detection limit （3S/N） of the method was 0. 004 mg · L^-1. Test for recovery was made by standard addition method at 3 concentration levels of 0. 01 mg · kg^-1, 0. 02 mg · kg^-1 and 0. 05 mg · kg^-1, and the results obtained were in the range of 70% to 115%, with values of RSD＇s （n= 6） less than 10. 2%.