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超高效液相色谱-串联质谱法检测婴儿米粉中11种有机磷阻燃剂

王溪 凌映茹 张昊 吉文亮

王溪,凌映茹,张昊,等. 超高效液相色谱-串联质谱法检测婴儿米粉中11种有机磷阻燃剂[J]. 食品工业科技,2022,43(17):301−308. doi:  10.13386/j.issn1002-0306.2021110236
引用本文: 王溪,凌映茹,张昊,等. 超高效液相色谱-串联质谱法检测婴儿米粉中11种有机磷阻燃剂[J]. 食品工业科技,2022,43(17):301−308. doi:  10.13386/j.issn1002-0306.2021110236
WANG Xi, LING Yingru, ZHANG Hao, et al. Determination of 11 Kinds of Organophosphorus Flame Retardants in Baby Rice Cereal by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(17): 301−308. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021110236
Citation: WANG Xi, LING Yingru, ZHANG Hao, et al. Determination of 11 Kinds of Organophosphorus Flame Retardants in Baby Rice Cereal by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(17): 301−308. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021110236

超高效液相色谱-串联质谱法检测婴儿米粉中11种有机磷阻燃剂

doi: 10.13386/j.issn1002-0306.2021110236
基金项目: 淮安市突发公共卫生事件应急检测重点实验室开放课题(ETPHI-K-04);江苏省医学重点学科(ZDXKA2016008)。
详细信息
    作者简介:

    王溪(1990−),女,硕士,主管技师,研究方向:食品、化妆品、消毒产品理化检验,E-mail:wangxi_sanjia@163.com

  • 中图分类号: TS201

Determination of 11 Kinds of Organophosphorus Flame Retardants in Baby Rice Cereal by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

  • 摘要: 采用超高效液相色谱-串联质谱技术,建立婴儿米粉中11种有机磷阻燃剂的检测方法。样品用0.5%甲酸乙腈溶液超声提取,提取液经分散固相萃取吸附剂净化,聚四氟乙烯滤膜过滤后上机检测,5 mmol/L甲酸铵的水溶液和乙腈为流动相梯度洗脱,目标化合物在ACQUITY UPLC® BEH C18 色谱柱(100 mm×2.1 mm,1.7 μm)上实现分离,在电喷雾正离子扫描模式下进行多反应监测(MRM),外标法定量。通过优化色谱条件,11种有机磷阻燃剂均达到了基线分离。11种有机磷阻燃剂在0.5~100 μg/L(磷酸三辛酯0.05~10 μg/L)范围内线性关系良好,相关系数r均大于0.994。检出限(3S/N)为0.003~0.926 μg/kg,定量限(10S/N)为0.01~2.78 μg/kg。婴儿米粉中低、中、高3个添加浓度水平的加标回收率为63.2%~113.4%,相对标准偏差(n=6)均小于10%。运用建立的方法分析了4种婴儿米粉,磷酸三苯酯的检出率高达100%,其中一份米粉检出了磷酸三正丁酯和磷酸三(2-氯丙基)酯。该方法简单可靠、灵敏度高、重现性好,覆盖的有机磷阻燃剂种类多,适用于婴儿米粉中痕量有机磷阻燃剂的检测。
  • 图  1  11种OPFRs标准溶液的提取离子流图

    Figure  1.  Extracted ion chromatograms of 11 kinds of OPFRs standard solutions

    注: TEHP浓度为2 μg/L,其余标准液浓度为20 μg/L。

    图  2  程序空白提取液过不同滤膜时TEP的检出情况

    Figure  2.  Detection of TEP when blank extract passed through different filter membrane

    注:A:空白提取液不过滤膜;B:空白提取液过尼龙滤膜;C:空白提取液过再生纤维素滤膜;D:空白提取液过PTFE滤膜。

    图  3  不同溶剂的提取效率

    Figure  3.  Extraction efficiency of different solvents

    注:A:0.5%甲酸乙腈;B:4:1乙腈丙酮;C:乙腈。

    图  4  不同净化管对OPFRs提取效率的影响

    Figure  4.  Effect of different purification pipes on extraction efficiency of OPFRs

    注:A、B、C分别对应A管、B管、C管。

    表  1  流动相梯度洗脱程序

    Table  1.   Gradient elution program for mobile phase

    时间(min)A相(%)B相(%)
    08020
    83565
    90100
    120100
    138020
    148020
    下载: 导出CSV

    表  2  目标化合物质谱参数

    Table  2.   Mass spectrometry parameters for the target OPFRs

    化合物CAS号保留时间(min)母离子(m/z)子离子
    (m/z)
    锥孔电压(V)碰撞能量(eV)
    TEP78-40-02.92183.199.0*/127.02016/12
    TiPP513-02-05.39225.199.0*/141.02016/9
    TnPP513-08-66.11225.199.0*/141.02016/9
    TiBP126-71-68.86267.199.0*/155.02017/10
    TnBP126-73-88.98267.199.0*/155.02017/10
    TCEP115-96-84.67287.099.0*/124.92022/22
    TPhP115-86-68.85327.177.0/152.0*2040/35
    TCPP13674-84-56.77328.199.0*/174.92018/12
    TBOEP78-51-39.49399.3199.0/299.0*2015/12
    TDCPP13674-87-88.47431.098.7*/320.82022/11
    TEHP78-42-212.13435.399.0*/323.22014/7
    注:“*”为定量离子
    下载: 导出CSV

    表  3  不同溶剂中OPFRs的响应

    Table  3.   Response of OPFRs in different solvents

    斜率TEPTiPPTnPPTiBPTnBPTCEPTPhPTCPPTBOEPTDCPPTEHP
    甲醇4.9×1052.3×1056.0×1053.2×1054.0×1059.0×1033.0×1048.5×1031.7×105620.28.5×105
    80%甲醇4.7×1053.1×1059.7×1053.4×1054.9×1051.0×1044.6×1041.1×1042.1×105839.11.2×106
    下载: 导出CSV

    表  4  11种OPFRs的检出限、定量限、线性相关系数及线性方程

    Table  4.   LOD, LOQ, linear correlation coefficient and linear equation of 11 kinds of OPFRs

    标准品线性范围(μg/L)线性方程相关系数rLOD
    (μg/kg)
    LOQ
    (μg/kg)
    TEP0.5~100y=384599.2x+257374.60.99970.6672.00
    TiPP0.5~100y=347665.9x−33966.80.99990.1110.33
    TnPP0.5~100y=598665.0x+38063.00.99970.0740.22
    TiBP0.5~100y=335398.2x+218614.40.99930.0420.13
    TnBP0.5~100y=467942.4x+188062.60.99990.0350.10
    TCEP0.5~100y=7415.2x+971.50.99980.9262.78
    TPhP0.5~100y=41675.4x+1812.30.99950.0930.28
    TCPP0.5~100y=8378.9x+16408.40.99910.6672.00
    TBOEP0.5~100y=177095.2x+55890.30.99980.0100.03
    TDCPP0.5~100y=737.7x+1667.80.99640.5561.67
    TEHP0.05~10y=1621194.8x+415578.80.99470.0030.01
    下载: 导出CSV

    表  5  婴儿米粉中OPFRs的加标回收率及相对标准偏差(n=6)

    Table  5.   Recovery rate and relative standard deviation of OPFRs in babyrice cereal (n=6)

    标准品加标量(μg/kg)
    10100500
    回收率(%)RSD(%)回收率(%)RSD(%)回收率(%)RSD(%)
    TEP65.55.685.82.192.46.9
    TiPP63.22.487.73.697.81.7
    TnPP68.86.394.03.8100.84.5
    TiBP86.87.299.83.4103.24.4
    TnBP81.39.899.55.1106.05.9
    TCEP74.68.691.33.497.93.6
    TPhP95.48.393.79.295.27.4
    TCPP81.43.294.16.9100.46.3
    TBOEP101.28.4105.57.7113.43.6
    TDCPP79.44.199.79.4102.86.1
    0.11050
    回收率(%)RSD(%)回收率(%)RSD(%)回收率(%)RSD(%)
    TEHP69.07.576.43.874.33.8
    下载: 导出CSV
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  • 收稿日期:  2021-11-19
  • 网络出版日期:  2022-07-17

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    《食品工业科技》青年编委专栏征稿 | 杂粮与主粮复配的营养学基础