食品科学 ›› 2024, Vol. 45 ›› Issue (1): 225-231.doi: 10.7506/spkx1002-6630-20230328-276

• 安全检测 • 上一篇    

超高效合相色谱法快速测定食品接触材料中9 种丙烯酸酯类化合物

邱月,谭超兰,刘小玉,陆嘉莉,余秋玲   

  1. (重庆市计量质量检测研究院,重庆 401123)
  • 发布日期:2024-02-05
  • 基金资助:
    国家市场监督管理总局科技计划项目(2023MK106);重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001); 重庆市市场监督管理局科研计划项目(CQSJKJ2022040;CQSJKJ2023003)

Rapid Determination of Nine Acrylates in Food Contact Materials by Ultra Performance Convergence Chromatography

QIU Yue, TAN Chaolan, LIU Xiaoyu, LU Jiali, YU Qiuling   

  1. (Chongqing Academy of Metrology and Quality Inspection, Chongqing 401123, China)
  • Published:2024-02-05

摘要: 采用超高效合相色谱(ultra performance convergence chromatography,UPC2)技术建立同时测定食品接触材料中9 种丙烯酸酯类化合物的快速分析方法。样品经甲醇超声萃取,过有机滤膜,采用超临界二氧化碳-乙腈为流动相进行梯度洗脱,选用超高效色谱柱ACQUITY UPC2 HSS C18 SB,采用二极管阵列检测器在210 nm波长处进行检测。结果表明,在最优条件(柱温40 ℃、背压13.79 MPa)下,9 种丙烯酸酯类化合物在4 min内可完成定性定量分析。甲基丙烯酸苯酯、甲基丙烯酸苯甲酯、乙二醇二甲基丙烯酸酯的线性范围为0.2~100 mg/L,甲基丙烯酸的线性范围为0.3~100 mg/L,丙烯酸丁酯、甲基丙烯酸羟乙酯、丙烯酸羟乙酯的线性范围为0.4~100 mg/L,甲基丙烯酸异丁酯、丙烯酸卞酯的线性范围为0.5~100 mg/L,9 种丙烯酸酯类化合物标准曲线的决定系数(R2)均高于0.998 5。在高(30 mg/kg)、中(6 mg/kg)、低(0.2、0.3、0.4、0.5 mg/kg)3 个加标水平下,9 种丙烯酸酯类化合物的加标回收率(n=6)为89.3%~109.7%,相对标准偏差为0.62%~3.86%,检出限(RSN≥3)为0.05~0.15 mg/kg,定量限(RSN≥10)为0.2~0.5 mg/kg。将所建方法应用于30 批次实际样品的检测,发现食品接触材料中存在丙烯酸酯类化合物残留风险。

关键词: 丙烯酸酯类化合物;超高效合相色谱;塑料;食品接触材料;超声萃取

Abstract: Ultra performance convergence chromatography (UPC2) was used to establish a rapid analytical method to determine nine acrylate compounds in plastic food contact materials simultaneously. The samples were extracted with methanol, filtered through an organic membrane, and separated on an ACQUITY UPC2 HSS C18 SB column with gradient elution using a mobile phase consisting of supercritical carbon dioxide and acetonitrile. The photodiode array (PDA) detector was set at 210 nm. Experimental results showed that under the optimal conditions (column temperature, 40 ℃; and back pressure, 13.79 MPa), qualitative and quantitative analysis of the nine acrylates was completed within 4 min. Linear ranges were 0.2–100 mg/L for phenyl methacrylate (PNMA), benzyl methacrylate (BZMA) and ethylene dimethacrylate (EDMA); 0.3–100 mg/L for methacrylic acid (MAA); 0.4–100 mg/L for butyl acrylate (BTA), hydroxyethyl methylacrylate (HEMA) and hydroxyethyl acrylate (HEA); and 0.5–100 mg/L for isobutylmeth acrylate (IBMA) and benzyl acrylate (BZA). The determination coefficients (R2) of the standard curves for all acrylates were higher than 0.998 5, and recoveries obtained at high (30 mg/kg), middle (6 mg/kg) and low (0.2, 0.3, 0.4 and 0.5 mg/kg) spiked concentrations ranged from 89.3% to 109.7%, with relative standard deviations of 0.62% to 3.86% (n = 6). The limits of detection (RSN ≥ 3) were 0.05–0.15 mg/kg, and the limits of quantification (RSN ≥ 10) were 0.2–0.5 mg/kg. The proposed method identified the risk of acrylate residues in 30 batches of actual samples.

Key words: acrylates; ultra performance convergence chromatography; plastic; food contact materials; ultrasonic extraction

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