建立了台湾青枣( Zizyphus mauritiana Lam)中炔螨特、戊唑醇和溴螨酯同时测定的气相色谱-串联质谱(GC-MS / MS)分析方法。样品用乙腈匀浆提取,盐析,石墨化炭黑/氨基混合型固相萃取柱净化,乙腈/甲苯(3:1, v / v)洗脱,浓缩定容后检测。目标化合物经 SLB-5MS 色谱柱(30 m×0.25 mm×0.25μm)分离,采用三重串联四极杆质谱多反应监测(MRM)模式进行定性定量分析。结果表明,在0.01~0.50 mg / kg 添加水平时,3种农药的回收率为75.8%~103.6%,相对标准偏差为1.7%~9.3%( n =5)。方法的线性范围为0.01~0.50 mg / kg,决定系数(R2)﹥0.99。该方法对炔螨特、戊唑醇和溴螨酯的定量限均为0.01 mg / kg,能满足台湾青枣中炔螨特、戊唑醇和溴螨酯残留检测的要求。
An analytical method was established for the determination of propargite,tebucon-azole and bromopropylate in Taiwan green jujubes( Zizyphus mauritiana Lam)by gas chro-matography-tandem mass spectrometry(GC-MS / MS). The sample was extracted with acetoni-trile from the Taiwan green jujubes after treated with a homogenizer. The organic phase was then separated from water phase by adding NaCl. The extract was further purified on a carbon /NH 2 cartridge with elution solvents of acetonitrile / toluene(3 :1,v / v). Finally,the target ana-lytes were separated by a capillary gas chromatographic column SLB-5MS( 30 m × 0. 25 mm × 0. 25 μm). A tandem quadrupole mass spectrometer operated in either full scan mode or in MS /MS mode for multiple reaction monitoring(MRM)was used for the qualitative and quantitative analysis of the constituents,respectively. The results showed that the average recoveries of the three pesticides ranged from 75. 8% to 103. 6% with the RSDs of 1. 7% -9. 3% at the spiking lev-els from 0. 01 mg / kg to 0. 50 mg / kg(n = 5). The calibration curves showed good linearity in the range of 0. 01-0. 50 mg / kg,with the determination coefficients over 0. 99(R 2﹥0. 99). The lim-its of quantification(LOQs)were 0. 01 mg / kg for propargite,tebuconazole and bromopropylate in Taiwan green jujubes. The method is available for the determination of propargite,tebucon-azole and bromopropylate pesticide residues in Taiwan green jujubes.
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