酰胺化衍生-高效液相色谱-四极杆-高分辨飞行时间质谱法测定食品接触塑料材料中7种烷基胺

引用本文: 区硕俊, 岑建斌, 梁俊发, 李秀英, 郭新东, 寻知庆, 罗曼妮, 曾广丰. 酰胺化衍生-高效液相色谱-四极杆-高分辨飞行时间质谱法测定食品接触塑料材料中7种烷基胺[J]. 分析化学, 2020, 48(3): 413-422. doi: 10.19756/j.issn.0253-3820.191049 shu

Citation: OU Shuo-Jun, CEN Jian-Bin, LIANG Jun-Fa, LI Xiu-Ying, GUO Xin-Dong, XUN Zhi-Qing, LUO Man-Ni, ZENG Guang-Feng. Determination of Seven Kinds of Alkylamines in Food Contact Plastic Materials by Amidation Coupled with High Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometer[J]. Chinese Journal of Analytical Chemistry, 2020, 48(3): 413-422. doi: 10.19756/j.issn.0253-3820.191049 shu

酰胺化衍生-高效液相色谱-四极杆-高分辨飞行时间质谱法测定食品接触塑料材料中7种烷基胺

1.
广州海关技术中心, 广东省动植物食品进出口措施研究重点实验室, 广州 510623;
2.
广州检验检测认证集团有限公司, 国家加工食品质量检验中心(广东), 广州 511447;
3.
广州质量监督检测研究院, 广州 511447
基金项目:
本文系国家质量监督检验检疫总局科技计划项目（No.2015QK162）

摘要: 建立了高效液相色谱-四极杆-高分辨飞行时间质谱法（HPLC-Q-TOF-MS）用于同时测定食品接触塑料材料中7种烷基胺。用0.4%氯甲酸苄酯的乙腈-Na₂CO₃溶液（50∶50，V/V）对样品进行酰胺化衍生，采用响应曲面实验设计优化的前处理衍生条件为：1.5%（m/V） Na₂CO₃溶液、氯甲酸苄酯（Cbz-Cl）比例为0.4%（V/V）、NaCl用量为1.5 g。衍生物在优化的色谱和质谱条件下，采用ESI源正离子扫描方式进行数据采集。在1.0~500 μg/L范围内，7种烷基胺的浓度与响应强度，呈良好线性关系，相关系数R²均大于0.9957，平均回收率为82.0%~108.0%，检出限为0.5~1.0 μg/kg，定量限为2.0~4.0 μg/kg，相对标准偏差为3.5%~6.8%。本方法具有操作简便、灵敏度高、重现性好和准确度高等优点，可用于分析测定食品接触塑料材料中7种烷基胺。

关键词:

English

Determination of Seven Kinds of Alkylamines in Food Contact Plastic Materials by Amidation Coupled with High Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometer

1.
Guangzhou Customs Technology Center, Guangzhou Key Laboratory of Import and Export Technical Measures of Animal, Plant and Food, Guangzhou 510623, China;
2.
Guangzhou Inspection and Certification Group Co. Ltd., Guangzhou 511447, China;
3.
Guangzhou Quality Supervision and Testing Institute, Guangzhou 511447, China
Received Date: 21 January 2019
Revised Date: 26 November 2019
Fund Project:
This work was supported by the Science and Technology Plan of General Administration of Quality Supervision, Inspection and Quarantine of the People`s Republic of China (No. 2015QK162).

Abstract: A high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF/MS) method for determination of seven kinds of alkylamines was established. Samples were amidated with 0.4% benzyl chloroformate (Cbz-Cl) in acetonitrile-sodium carbonate solution (50:50, V/V). The amidated conditions, including concentration of sodium carbonate solution (1.5%, m/V), benzyl chloroformate ratio and amount of sodium chloride (1.5 g), were optimized by response surface methodology. Under the optimized chromatographic and mass spectrometer conditions, the data were collected with electrospray ionization (ESI) sources under positive ion mode. The calibration curves of seven kinds of alkylamines showed good linearity in concentration range of 1.0-500 μg/L(R²>0.9957). The average recoveries were 82.0%-108.0%, the limits of detection and quantification were 0.5-1.0 μg/kg and 2.0-4.0 μg/kg, respectively, and the relative standard deviations (RSDs) were 3.5%-6.8%. This method is efficient and easy to be operated, and has good sensitivity, high precision and accuracy in the determination of seven alkylamines in food contact plastic materials.

Key words:

High performance liquid chromatography-quadrupole time-of-flight mass spectrometry
/ Alkylamines
/ Amidated
/ Response surface methodology
/ Food contact plastic materials

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沈阳化工大学材料科学与工程学院沈阳 110142

酰胺化衍生-高效液相色谱-四极杆-高分辨飞行时间质谱法测定食品接触塑料材料中7种烷基胺

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Determination of Seven Kinds of Alkylamines in Food Contact Plastic Materials by Amidation Coupled with High Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometer

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