静态顶空气相色谱-质谱联用法同时测定食品添加剂中9种有机溶剂残留

Simultaneous Determination of 9 Residual Organic Solvents in Food Additives by Static Headspace Gas Chromatography-Mass Spectrometry

建立一种用于食品添加剂中常见的9种残留溶剂含量的顶空气相色谱-质谱联用检测方法,对顶空孵化温度、孵化时间的影响进行研究。结果表明:孵化温度在80℃、孵化时间5 min时,选用HP-5MS(30m×0.25mm,0.25μm)的毛细管色谱柱对9种有机溶残在10 min内能很好地分离。该法在烷烃类、芳香烃类有机溶剂在0.1~10 mg/L、酯类、酮类1.0~100 mg/L、醇类4.0~400 mg/L范围内线性关系良好,9种残留溶剂的相关系数均大于0.9971,加标回收率87.54%~106.50%,相对标准偏差(n=5)1.43%~6.17%。检出限范围为烷烃类、芳香烃类0.0004~0.0052 mg/L;酯类、酮类0.0160~0.0240 mg/L;醇类0.5500~0.5960 mg/L。该法快速、准确、灵敏度高,适用于食品添加剂中多种溶剂残留量的同时测定。

An analytical method was developed for the determination of 9 residual solvents in food additives by static headspace gas chromatography-mass spectrometry(HS-GC-MS). The optimal chromatographic conditions were as follows: an HP-5MS capillary column(30 m × 0.25 mm, 0.25 μm), and equilibration of the sample in the headspace vessel at 80 ℃ in 5 min. The results showed that all 9 organic residues were separated well within 10 min, and the standard curves were linear in the range of 0.1–10 mg/L for alkanes and aromatic hydrocarbons, 1–100 mg/L for esters and ketones, and 4.0–400 mg/L for alcohols. The correlation coefficients were more than 0.9971 for 9 residual organic solvents. The recoveries for spiked samples were 87.54%–106.50% with RSD(n = 5) in the range of 1.43%–6.17%, and the limits of detection were 0.0004–0.0052 mg/L for alkanes and aromatic hydrocarbons, 0.0160–0.0240 mg/L for esters and ketones, and 0.5500–0.5960mg/L for alcohols. The proposed method is simple, rapid, sensitive and accurate, and can be used for the simultaneous determination of residual solvents in food additives.