高效液相色谱—串联质谱法测定食品塑料包装材料中双酚A和壬基酚
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(湖南省产商品质量检验研究院,湖南 长沙 410007)

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唐吉旺(1980—),男,湖南省产商品质量检验研究院高级工程师,博士。E-mail: feifeinvzi@126.com

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湖南省市场监督管理局科技计划项目(编号:2019KJJH10)


Determination of bisphenol A and nonylphenol in food packaging material by high performance liquid chromatography-tandem mass spectrometry
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(The Product and Commodity Quality Supervison and Inspection Institute of Hunan Province, Changsha, Hunan 410007, China)

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    摘要:

    目的:基于高效液相色谱—串联质谱技术,建立一种检测食品包装材料中双酚A和壬基酚的方法。方法:用不同的提取溶剂和提取方法提取标准样品中的双酚A和壬基酚,以目标物的提取量为指标确定最佳提取溶剂和提取方法,在此基础上考察固相萃取柱、上样溶剂、淋洗溶剂及洗脱溶剂对净化效果的影响。样品以二氯甲烷为溶剂超声提取后经硅胶固相萃取柱净化,用Venusil MP C18(2)色谱柱(100 mm×2.1 mm,2.6 μm)进行分离,以0.1%氨水和甲醇为流动相进行梯度洗脱,在ESI负离子扫描模式下采用多反应监测模式测定,内标法定量。结果:双酚A和壬基酚在1.0~200.0 μg/L范围内均具有良好的线性关系,相关系数R>0.999,在1.0,10.0,200.0 μg/kg 3个加标水平下的平均回收率为89.2%~101.2%,相对标准偏差(RSD)为3.1%~6.2%。方法的检测限和定量限分别为0.5,1.0 μg/kg。结论:该方法操作简单、准确、灵敏,可适用于食品包装材料中双酚A和壬基酚含量的测定。

    Abstract:

    Objective: A method based on high-performance liquid chromatography-mass spectrometry was developed for the simultaneous determination of bisphenol A and nonylphenol in food packaging material. Methods: The extraction solvent and extraction method were investigated. Solid-phase extraction (SPE) conditions were optimized. The effects of solid phase extraction column, loading solvent, eluting solvent and elution solvent on the purification effect were systematically analyzed. The samples were ultrasonic extracted with dichloromethaneand cleaned up on a solid-phase extraction (SPE) cartridge equipped with packing material of silicone. The separation was performed on a Venusil MP C18(2)(100 mm×2.1 mm,2.6 μm)by gradient elution with 0.1% ammonia solution and methanol as mobile phase. The analytes were determined with multiple reaction monitoring (MRM) mode under electrospray negative ionization mode and quantified by an internal standard method. Results: The results indicated that good linearities was obtained for bisphenol A and nonylphenol both within the concentration range of 1.0~200.0 μg/L. The average recoveries of each analyte at three spiked levels of 1.0, 10.0, 200.0 μg/kg were in the range of 89.2%~101.2%, with relative standard deviations (RSD) of 3.1%~6.2%. The limits of detection (LODs) and limits of quantification (LOQs) were 0.5 μg/kg and 1.0 μg/kg, respectively. Conclusion: The method was proved to be a simple, accurate and sensitive method and was successfully applied to detect bisphenol A and nonylphenol in food packaging material. It can also provide reference for the determination of bisphenol A and nonylphenol in food.

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唐吉旺,袁列江,肖 泳,等.高效液相色谱—串联质谱法测定食品塑料包装材料中双酚A和壬基酚[J].食品与机械,2023,39(1):37-41.
TANG Ji-wang, YUAN Lie-jiang, XIAO Yong, et al. Determination of bisphenol A and nonylphenol in food packaging material by high performance liquid chromatography-tandem mass spectrometry[J]. Food & Machinery,2023,39(1):37-41.

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  • 收稿日期:2022-05-31
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  • 在线发布日期: 2023-04-25
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