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气相色谱-质谱法测定植物油中壬基酚含量
Determination of 4-nonylphenol in vegetable oil by gas chromatography-mass spectrometry
【摘要】 目的建立气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)检测植物油中壬基酚(4-nonylphenol,4-NP)的分析方法,了解市售植物油中壬基酚的污染状况。方法样品加入乙腈提取液,超声提取、固相萃取柱净化、七氟丁酸酐衍生化后,采用GC-MS进行检测,同位素内标法定量。结果在线性范围5~200μg/kg内,方法回归方程为Y=7.78×10-3X,相关系数为0.9991。方法的检出限为3.0μg/kg,定量限9.8μg/kg。加标回收率范围为75.7%~107.4%,相对标准偏差(relative standard deviation, RSD)为5.5%~9.7%。共检测50份市售植物油样品,其中26份植物油样品检出4-NP,检出率为52%,含量范围为3.21~28.2μg/kg,中位值为3.63μg/kg。结论此方法灵敏度较高,可用于植物油中4-NP的准确定量。检测数据表明,植物油样品壬基酚检出率较高,因此对其含量的监测不容忽视。
【Abstract】 Objective To establish a method for the determination of 4-nonylphenol(4-NP) in vegetable oil by gas chromatography-mass spectrometry(GC-MS), and to understand the pollution status of 4-NP in vegetable oil. Methods The samples were extracted with acetonitrile by ultrasound, purified by solid phase extraction column, and derivatized with heptafluorobutyric anhydride. The samples were detected by GC-MS and quantified by isotope internal standard method. Results In the linear range of 5-200 μg/kg, the regression equation was Y=7.78×10-3X, and the correlation coefficient was 0.9991. The limit of detection was 3.0 μg/kg and the limit of quantitation was 9.8 μg/kg. The recoveries ranged from 75.7% to 107.4%, and the relative standard deviations(RSDs) ranged from 5.5% to 9.7%. Totally 50 commercial vegetable oil samples were detected, 4-NP was detected in 26 samples, the detection rate was 52%, the content range was 3.21-28.2 μg/kg, and the median value was 3.63 μg/kg. Conclusion This method is simple and sensitive, and can be used for the accurate determination of 4-NP in vegetable oil. The detection data showes that the detection rate of nonylphenol in vegetable oil samples is high, so the monitoring of its content should not be ignored.
【Key words】 4-nonylphenol; vegetable oil; derivatization; isotope internal standards; gas chromatography-mass spectrometry;
- 【文献出处】 食品安全质量检测学报 ,Journal of Food Safety & Quality , 编辑部邮箱 ,2021年05期
- 【分类号】O657.63;TS225.1
- 【被引频次】4
- 【下载频次】140