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

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0.5mL,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,r^2>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。

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,r^2>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.