顶空气相色谱-质谱法同时测定蜂蜜中57种挥发性有机溶剂残留

建立了顶空气相色谱-质谱(HS-GC/MS)同时测定蜂蜜中57种挥发性有机溶剂(包括烷烃类、芳香烃类、醇类、酮类、酯类、醚类)残留量的分析方法。蜂蜜样品在密封的顶空瓶中用水溶解后,在顶空仪中于80 ℃下平衡30 min,使气-液两相达到动态平衡。采用DB-624毛细管色谱柱(60 m×0.25 mm×1.40 μm)对57种有机溶剂进行分离,GC/MS测定,外标法定量。该方法对于烷烃类、芳香烃类和醚类挥发性有机溶剂在0.005～0.2 μg、酯类0.05～2.0 μg、酮类0.5～20 μg、醇类2.5～100 μg范围内线性关系良好,相关系数均大于0.996。对于烷烃类、芳香烃类和醚类挥发性有机溶剂在1.0～20 μg/kg、酯类10～200 μg/kg、酮类100～2000 μg/kg、醇类500～10000 μg/kg添加范围内的平均添加回收率为61.0%～113.1%,相对标准偏差为1.9%～9.8%。对于烷烃类、芳香烃类和醚类挥发性有机溶剂的检出限为1.0 μg/kg、酯类10 μg/kg、酮类100 μg/kg、醇类500 μg/kg。该方法操作简单、快速,灵敏度和准确度高,适用于蜂蜜样品中多种挥发性有机溶剂残留量的同时检测。

Simultaneous determination of 57 residual volatile organic solvents in honey by headspace gas chromatography-mass spectrometry

A method was developed for the simultaneous determination of 57 residual volatile organic solvents (including several alkanes, aromatic hydrocarbons, alcohols, ketones, esters and ethers) in honey by headspace gas chromatography-mass spectrometry (HS-GC/MS). The honey sample was dissolved with water in a headspace vial, and the equilibration of the sample in the headspace vessel was achieved at 80 ℃ in 30 min. A DB-624 capillary chromatographic column (60 m×0.25 mm×1.40 μm) was used for the separation of 57 volatile organic solvents, and the analysis was performed by GC/MS. The external calibrations were used for the quantification. The linear ranges of the method were 0.005~0.2 μg for the alkanes, aromatic hydrocarbons and ethers, 0.05~2.0 μg for the esters, 0.5~20 μg for the ketones, 2.5~100 μg for the alcohols. The correlation coefficients were more than 0.996 for all the volatile organic solvents. The recoveries and the relative standard deviations were from 61.0% to 113.1% and 1.9% to 9.8%, respectively, at the spiked levels of 1.0~20 μg/kg for the alkanes, aromatic hydrocarbons and ethers, 10~200 μg/kg for the esters, 100~2000 μg/kg for the ketones, 500~10000 μg/kg for the alcohols. The limits of detection were 1.0 μg/kg for the alkanes, aromatic hydrocarbons and ethers, 10 μg/kg for the esters, 100 μg/kg for the ketones, 500 μg/kg for the alcohols. The method is simple, rapid, sensitive and accurate, and can be used for the simultaneous determination of residual volatile organic solvents in honey samples.