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建立了黄瓜和番茄中毒氟磷残留量的固相萃取-气相色谱-质谱联用(SPE-GC-MS)分析方法;对毒氟磷的裂解机理进行了探讨,确定了测试分析的定性离子和定量离子。样品采用V(正己烷)∶V(丙酮)=1∶1混合液高速匀浆提取,使用以N-丙基乙二胺(PSA)、C18和石墨化炭黑(GCB)的混合物为填料的固相萃取柱净化,采用气相色谱-质谱联用仪在选择离子扫描(SIM)模式下进行检测,外标法定量。结果显示,毒氟磷在0.01~0.5 mg/L内,标准溶液的峰面积与质量浓度的线性关系良好(r≥0.999),方法的检出限(LOD)(S/N=3)为0.003 mg/kg,定量限(LOQ)(S/N=10)为0.01 mg/kg。在0.01、0.02和0.1 mg/kg添加水平下,毒氟磷的平均回收率为99.9%~100.2%,相对标准偏差(RSD,n=6)为0.97%~3.07%。
A SPE-GC-MS method was developed for the determination of the amount of residual fluorine and phosphorus in cucumber and tomato. The mechanism of cleavage of toxic fluorine and phosphorus was discussed, and the qualitative analysis of the ions and Quantitative ion. The samples were homogenized by high speed homogenization with V (n-hexane): V (acetone) = 1: 1 using a mixture of N-propyl ethylenediamine (PSA), C18 and graphitized carbon black The solid phase extraction column was cleaned and detected by gas chromatography-mass spectrometry in a selective ion scan (SIM) mode and quantified by external standard method. The results showed that the linear range of the standard solution peak area was linear (r≥0.999) and the limit of detection (LOD) (S / N = 3) was 0.003 mg / kg, and the limit of quantification (LOQ) (S / N = 10) was 0.01 mg / kg. The average recovery of toxic fluorine was 99.9% ~ 100.2% with relative standard deviations (RSD, n = 6) of 0.97% ~ 3.07% at the 0.01, 0.02 and 0.1 mg / kg loading levels.