食品科学

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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

洪 华,王 莉,武中平,顾爱国,王 伟   

  1. 江苏省产品质量监督检验研究院,江苏 南京 210007
  • 出版日期:2014-09-25 发布日期:2014-09-17

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

HONG Hua, WANG Li, WU Zhong-ping, GU Ai-guo, WANG We   

  1. Jiangsu Provincial Supervising and Testing Research Institute for Products Quality, Nanjing 210007, China
  • Online:2014-09-25 Published:2014-09-17

摘要:

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(30 m×0.25 mm,0.25 μm)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0.997 1,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0.000 4~0.005 2 mg/L;酯类、酮类0.016 0~0.024 0 mg/L;醇类0.550 0~0.596 0 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。

关键词: 顶空, 气相色谱-质谱, 有机溶剂, 残留, 食品添加剂

Abstract:

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 0.997 1 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 0.000 4–0.005 2 mg/L for alkanes and aromatic hydrocarbons, 0.016 0–0.024 0 mg/L for esters and ketones,
and 0.550 0–0.596 0 mg/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.

Key words: headspace, gas chromatography-mass spectrometry, organic solvents, residual, food additive

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