顶空气相色谱法测定甘蓝中硫酰氟残留

Determination of sulfuryl fluoride residues in cabbage by headspace gas chromatography

中文关键词:  硫酰氟  甘蓝  顶空气相色谱法  残留

英文关键词:sulfonyl fluoride  cabbage  headspace gas chromatography  residue

中文摘要:

      目的 建立顶空气相色谱法(headspace gas chromatography, HS-GC)测定甘蓝中硫酰氟残留量的分析方法。方法 样品均质后, 采用顶空毛细管气相色谱法测定, 进样口温度: 150℃, 进样量 0.5 mL, 分流比20:1, 柱温: 70 ℃, 检测器温度: 250 ℃, 载气: N2, 外标法定量分析。结果 硫酰氟在0.001~1.000 mg/L范围内线性关系良好, r2>0.99, 方法检出限为0.001 mg/kg, 定量限为0.005 mg/kg。在0.005、0.05、0.1 mg/kg的添加水平下, 硫酰氟在甘蓝中的回收率为71%~116%, 相对标准偏差为7%~13%。结论 该方法该法操作简便, 重现性好, 结果准确可靠, 可以用于甘蓝中硫酰氟残留的测定。

英文摘要:

      Objective To establish a method for determination of sulfuryl fluoride residues in cabbage by headspace gas chromatography (HS-GC). Methods After homogenization, the sample was determined by headspace capillary gas chromatography. The temperature of the sample inlet was 150 ℃, the sample volume was 0.5 mL, the split ratio was 20:1, the column temperature was 70 ℃, the temperature of detector was 250 ℃, the carrier gas was N2, and the external standard was used forquantitative analysis. Results When the concentration was in the range of 0.001–1.000 mg/L, the linear relationship of sulfuryl fluoride was good, r2>0.99, the limit of detection was 0.001 mg/kg, and the limit of quantitation was 0.005 mg/kg. The recoveries of sulfuryl fluoride in cabbage samples at 3 spiked levels of 0.005, 0.05 and 0.1 mg/kg were ranged from 71%–116% and the relative standard deviations were 7%–13%. Conclusions This method is simple, accurate and reproducible, which is suitable for quantitative analysis of sulfuryl fluoride in cabbage.