色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 111-115.DOI: 10.3724/SP.J.1123.2018.08009

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法同时测定果蔬清洗剂中12种防腐剂和抗氧化剂

蔡立鹏, 吕晓飞, 张蓓, 李小英, 赵晓甫   

  1. 河北省环保产品质量监督检验研究院, 国家环保产品质量监督检验中心, 河北 石家庄 050091
  • 收稿日期:2018-08-06 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 蔡立鹏,Tel:(0311)67568416,E-mail:tielang200@163.com.
  • 基金资助:

    河北省质量技术监督局科技计划（2016ZD07）.

Simultaneous determination of 12 preservatives and antioxidants in fruit and vegetable detergents by gas chromatography-mass spectrometry

CAI Lipeng, LÜ Xiaofei, ZHANG Bei, LI Xiaoying, ZHAO Xiaofu   

  1. Hebei Provincial Research Institute of Environmental Protection Products Quality Supervision and Inspection, China National Center for Quality Supervision and Test of Environmental Protection Products, Shijiazhuang 050091, China
  • Received:2018-08-06 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Science and Technology Plan of Hebei Provincial Administration of Quality and Technical Supervision (No. 2016ZD07).

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摘要：

建立了气相色谱-质谱同时检测果蔬清洗剂中12种防腐剂和抗氧化剂的方法。果蔬清洗剂样品先加入乙醇，经旋转蒸发除去样品中的水分，然后用正己烷饱和的乙腈溶液提取，饱和氯化钠溶液洗涤净化，净化后的样品溶液浓缩后用乙腈定容。被测组分经HP-5MS UI石英毛细管色谱柱（30 m×0.25 mm×0.25 μm）分离后在选择离子监测模式下测定。12种防腐剂和抗氧化剂在0.1~10 mg/L范围内线性关系良好，相关系数（r2）>0.999；检出限和定量限分别为0.010~0.030 mg/kg和0.030~0.090 mg/kg。按照建立的方法进行0.2、2.0和10 mg/kg 3个添加水平的加标回收试验，回收率为68.3%~115.3%，相对标准偏差为3.1%~11.3%。该法灵敏度高，定性准确，前处理净化效果好，适用于果蔬清洗剂中防腐剂和抗氧化剂的检测。

关键词: 防腐剂, 果蔬清洗剂, 抗氧化剂, 气相色谱-质谱

Abstract:

A method was established for the simultaneous determination of 12 preservatives and antioxidants in fruit and vegetable detergents by gas chromatography-mass spectrometry (GC-MS). First, ethanol was added to remove the water in the sample by rotary evaporation and was extracted with acetonitrile in saturated n-hexane. Finally, the residual surfactant in the sample solution was removed with a saturated sodium chloride solution. The purified sample solution was concentrated and metered volume by acetonitrile. The preservatives and antioxidants were separated on a HP-5MS UI capillary column (30 m×0.25 mm×0.25 μm), and detected in the selective ion monitoring (SIM) mode. The method had a good linearity in the range of 0.1-10 mg/L with correlation coefficients (r2)>0.999, and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.010-0.030 mg/kg and 0.030-0.090 mg/kg, respectively. The recoveries of the 12 preservatives and antioxidants at three spiked levels (0.2, 2.0 and 10 mg/kg) were 68.3%-115.3% with the relative standard deviations (RSDs) of 3.1%-11.3%. (n=7) The method is sensitive and accurate, and can be suitable for the determination of preservatives and antioxidants in fruit and vegetable detergents.

Key words: antioxidants, fruit and vegetable detergents, gas chromatography-mass spectrometry (GC-MS), preservatives

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