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加速溶剂提取-气相色谱-质谱法分析土壤和沉积物中15种有机磷酸酯类阻燃剂

潘萌, 佟玲, 田芹, 宋淑玲

潘萌,佟玲,田芹,等. 加速溶剂提取-气相色谱-质谱法分析土壤和沉积物中15种有机磷酸酯类阻燃剂[J]. 岩矿测试,2023,42(6):1165−1176. DOI: 10.15898/j.ykcs.202305110065
引用本文: 潘萌,佟玲,田芹,等. 加速溶剂提取-气相色谱-质谱法分析土壤和沉积物中15种有机磷酸酯类阻燃剂[J]. 岩矿测试,2023,42(6):1165−1176. DOI: 10.15898/j.ykcs.202305110065
PAN Meng,TONG Ling,TIAN Qin,et al. Determination of 15 Organophosphate Ester Flame Retardants in Soils and Sediments by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis,2023,42(6):1165−1176. DOI: 10.15898/j.ykcs.202305110065
Citation: PAN Meng,TONG Ling,TIAN Qin,et al. Determination of 15 Organophosphate Ester Flame Retardants in Soils and Sediments by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis,2023,42(6):1165−1176. DOI: 10.15898/j.ykcs.202305110065

加速溶剂提取-气相色谱-质谱法分析土壤和沉积物中15种有机磷酸酯类阻燃剂

基金项目: 中国地质调查局地质调查项目(DD20190475)
详细信息
    作者简介:

    潘萌,硕士,工程师,主要从事有机分析与检测。E-mail:spmile3629@163.com。

    通讯作者:

    佟玲,硕士,正高级工程师,主要从事环境有机污染物分析方法研究与应用。E-mail:winter_tl@sina.com

  • 中图分类号: S151.95;O657.63

Determination of 15 Organophosphate Ester Flame Retardants in Soils and Sediments by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction

  • 摘要:

    有机磷酸酯类阻燃剂广泛存在于环境中,长期接触会对生物体的生殖系统、免疫系统造成破坏,进而对人类健康产生影响,调查研究其在环境中的污染水平非常有必要,而多组分、同时、准确的分析技术是研究的基础,目前已有的分析方法在化合物种类和提取效率方面还有待提高。本文建立了一种分析土壤和沉积物中15种有机磷酸酯类阻燃剂的方法。新鲜样品采用加速溶剂萃取(ASE)直接提取,提取液用复合填料的固相萃取柱进行净化,再采用气相色谱-质谱(GC-MS)进行定性、定量分析。为了改善提取效率和净化效果等问题,针对土壤和沉积物样品基质的复杂性,实验中主要优化了样品的提取、净化条件:针对磷酸三(2-氯乙基)酯提取回收率低的问题,改进了样品制备方式,新鲜样品在有少量水的存在下直接提取,使得有机溶剂更好地与样品颗粒进行接触,显著提高了该化合物的提取效率;采用石墨化碳和氨基硅胶复合填料的固相萃取小柱对样品提取液进行净化,保障了复杂沉积物样品净化效果的有效性,同时选用5%甲苯的洗脱溶剂体系,能够提高磷酸三甲苯酯(TCP)在石墨化碳固相萃取柱上的洗脱效率,保证了净化过程的回收率。结果表明,目标化合物浓度在10.0~500.0ng/mL之间的标准曲线R2大于0.9962,5个添加水平下的平均回收率在72.6%~112.9%之间,相对标准偏差RSD(n=4)≤25.3%,方法检出限为0.17~1.21ng/g。采用该方法分析美国NIST有证标准物质,测试结果均在不确定度范围内。通过8家实验室验证表明该方法的各项指标满足分析测试要求,能够应用于土壤和沉积物等基质复杂的固体样品中有机磷酸酯类阻燃剂的分析。

  • 图  1   不同样品制备方法提取回收率的比较

    Figure  1.   Comparison of extraction recoveries of different sample preparation methods.

    图  2   不同提取溶剂条件下OPFRs目标化合物提取回收率比较

    Figure  2.   Comparison of recoveries by different extraction solvents for target compounds of OPFRs.

    图  3   不同提取温度下OPFRs目标化合物提取回收率比较

    Figure  3.   Comparison of recoveries by different extraction temperatures for target compounds of OPFRs.

    表  1   各OPFRs目标化合物保留时间及质谱参数

    Table  1   Retention times and mass spectrum parameters of target OPFRs .

    化合物名称(缩写)
    Compound name (Abbr.)
    保留时间
    Retention time (min)
    定量离子
    Quantitative ion (m/z)
    定性离子
    Qualitative ion (m/z)
    内标分组
    Internal standard grouping
    磷酸三乙酯(TEP)6.87515599,1271
    萘-D87.750136108,1371
    磷酸三丙酯(TPrP)9.50799141,1831
    苊-D1010.625162164,1602
    磷酸三异丁酯(TiBP)10.67999139,1552
    磷酸三丁酯-D27(TBP-D27)11.627167103,2312
    磷酸三正丁酯(TnBP)11.772155211,992
    磷酸三(2-氯乙基)酯(TCEP)12.760249143,205,2233
    磷酸三(2-氯丙基)酯(TCPP)*13.066277157,201,1253
    菲-D1013.222188184,1603
    磷酸三(1,3-二氯异丙基)酯(TDCP)17.101381321,1913
    磷酸三(丁氧基乙基)酯(TBEP)17.537199299,1533
    磷酸三苯酯-D15(TPP-D15)17.582341339,243,2233
    磷酸三苯酯(TPhP)17.645326325,215,1693
    2-乙基己基二苯基磷酸酯(DPEHP)17.770251250,170,943
    磷酸三辛酯(TEHP)17.89399113,2113
    䓛-D1218.347240236,2413
    三苯基氧膦(TPPO)18.679277278,199,1834
    邻位-磷酸三甲苯酯(o-TCP)19.079368277,1654
    间位-磷酸三甲苯酯(m-TCP)19.697368261,1654
    对位-磷酸三甲苯酯(p-TCP)20.789368261,1654
    注:“*”表示该化合物有两个色谱峰,需合并峰面积进行定量。
    下载: 导出CSV

    表  2   不同净化吸附剂OPFRs目标化合物的回收率比较

    Table  2   Comparison of the average recoveries by different adsorbents for target compounds of OPFRs.

    化合物
    Compounds
    石墨化碳(GCB)回收率
    Recovery of graphitized
    carbon (%)
    活性炭(C) 回收率
    Recovery of activated
    carbon (%)
    化合物
    Compound
    石墨化碳(GCB)回收率
    Recovery of graphitized
    carbon (%)
    活性炭(C) 回收率
    Recovery of activated
    carbon (%)
    TEP103.0- TPP-D15103.64.5
    TPrP96.5-TPhP93.16.1
    TiBP133.1125.6DPEHP103.349.9
    TBP-D2785.0119.8TEHP93.8172.1
    TnBP94.5125.1TPPO120.883.8
    TCEP96.9126.0o-TCP84.67.2
    TCPP85.8127.4m-TCP76.85.0
    TDCP116.2127.8p-TCP59.13.8
    TBEP135.3224.9
    注:“-”表示存在严重干扰,无法给出定量结果。
    下载: 导出CSV

    表  3   采用不同洗脱溶剂OPFRs目标化合物平均回收率

    Table  3   Average recoveries by different elution solvents for target compounds of OPFRs.

    化合物
    Compounds
    正己烷-丙酮(V/V)平均回收率
    Recovery of HEX-AC(V/V)(%)
    正己烷-丙酮(V/V,8∶2)平均回收率
    Recovery of HEX-AC(V/V,8∶2)(%)
    正己烷-丙酮(V/V,1∶1)平均回收率
    Recovery of HEX-AC(V/V,1∶1)(%)
    9∶18∶21∶11%甲苯
    1% Toluene
    3%甲苯
    3% Toluene
    5%甲苯
    5% Toluene
    1%甲苯
    1% Toluene
    3%甲苯
    3% Toluene
    5%甲苯
    5% Toluene
    TEP 99.9 123.1 114.8 99.7 104.7 108.9 114.2 109.8 121.1
    TPrP 51.3 84.5 84.9 67.2 78.5 87.2 79.3 77.8 85.1
    TiBP 119.8 107.7 107.2 92.6 102.0 123.6 96.1 95.7 111.4
    TBP-D27 91.3 106.7 106.3 81.2 100.1 108.7 99.9 96.8 106.8
    TnBP 88.4 94.3 96.3 68.3 88.3 91.8 90.3 85.7 101.2
    TCEP 131.4 128.3 133.3 107.2 120.6 121.4 125.3 115.5 130.4
    TCPP 100.9 96.8 102.1 85.5 97.0 97.1 96.7 95.5 99.7
    TDCP 98.9 106.1 101.4 78.8 100.9 95.7 98.6 87.9 99.8
    TBEP 100.5 96.8 98.3 67.0 100.0 95.3 102.0 89.6 118.0
    TPP-D15 93.1 103.7 100.9 77.4 93.1 91.9 97.7 84.8 96.8
    TPhP 91.0 91.8 96.7 97.3 93.0 93.6 101.7 91.9 98.5
    DPEHP 96.7 103.0 102.7 104.3 100.8 104.2 113.3 101.8 113.0
    TEHP 117.4 118.9 109.9 100.1 109.9 127.1 117.3 100.5 120.0
    TPPO 55.0 60.9 62.1 63.2 62.8 64.7 61.0 62.1 61.8
    o-TCP 82.2 90.3 91.7 97.7 89.4 90.9 98.9 91.2 95.4
    m-TCP 4.0 73.2 97.3 97.9 94.3 96.3 103.3 94.3 97.7
    p-TCP 0.0 0.0 13.8 5.5 91.6 99.9 71.3 98.6 103.1
    下载: 导出CSV

    表  4   OPFRs目标化合物精密度平均添加回收率、相对标准偏差及方法检出限

    Table  4   Average recoveries, RSD and detection limits of the method for target compounds of OPFRs.

    化合物
    Compounds
    平均添加回收率(相对标准偏差)
    Average recovery and RSD (%,n=4)
    最低添加浓度
    Minimum spiked level
    (ng/g)
    方法检出限
    MDL
    ( ng/g,n=7)
    2.0ng/g5.0ng/g10.0ng/g50.0ng/g500.0ng/g
    TEP 84.6 (15.7) 89.6 (6.9) 72.6 (8.3) 95.7 (4.8) 89.7 (1.8) 2.0 0.99
    TPrP 93.1 (11.4) 102.0 (4.1) 87.4 (4.1) 99.5 (5.1) 94.3 (2.6) 1.0 0.30
    TiBP 92.5 (17.1) 99.5 (4.4) 88.6 (4.3) 93.6 (7.5) 87.6 (6.6) 2.0 1.19
    TnBP 80.9 (25.3) 105.3 (12.2) 103.8 (11.7) 100.7 (5.8) 96.4 (3.4) 1.0 0.58
    TCEP 84.4 (7.4) 98.3 (4.8) 83.5 (9.9) 93.1 (6.9) 89.0 (3.0) 2.0 0.51
    TCPP 91.0 (18.3) 100.4 (9.9) 103.6 (8.7) 99.7 (5.3) 96.9 (1.6) 1.0 0.60
    TDCP 77.6 (3.9) 97.4 (5.6) 102.4 (4.1) 106.0 (6.8) 103.8 (1.9) 2.0 1.21
    TBEP 81.8 (5.1) 98.4 (7.7) 98.0 (6.2) 109.3 (14.9) 100.1 (5.6) 2.0 1.01
    TPhP 84.4 (5.2) 95.3 (2.6) 87.7 (4.3) 104.6 (5.4) 108.0 (4.5) 2.0 0.60
    DPEHP 88.2 (5.6) 97.7 (3.5) 95.5 (5.5) 112.9 (6.5) 95.8 (3.3) 1.0 0.21
    TEHP 84.1 (7.5) 99.6 (3.7) 92.9 (8.3) 108.6 (5.3) 102.1 (3.4) 2.0 0.45
    TPPO 85.6 (6.4) 75.7 (3.1) 74.1 (14.2) 111.5 (5.5) 99.2 (3.3) 2.0 0.40
    o-TCP 85.1 (7.9) 98.1 (3.4) 88.7 (3.3) 104.4 (5.1) 100.2 (5.0) 1.0 0.17
    m-TCP 87.4 (7.3) 95.3 (2.8) 91.0 (5.0) 105.3 (5.0) 93.8 (3.8) 1.0 0.35
    p-TCP 90.0 (11.4) 87.5 (4.9) 92.4 (5.9) 109.6 (7.6) 98.2 (2.6) 1.0 0.27
    TBP-D27 84.7 (9.1) 95.8 (3.5) 94.7 (6.3) 105.0 (4.8) 99.6 (3.3) - -
    TPP-D15 90.0 (16.3) 91.9 (4.0) 90.1 (4.0) 114.3 (7.0) 102.1 (3.5) - -
    注:“-”表示替代物无此项参数。
    下载: 导出CSV

    表  5   方法精密度统计结果

    Table  5   Statistical results of precision test for the method.

    化合物
    Compounds
    水平范围m
    Range of the level
    (ng/g)
    重复性限
    Repeatability limit
    r
    再现性限
    Reproducibility limit
    R
    TEP1.79~423r=0.1926+0.0217mR=0.3932+0.3338m
    TPrP1.78~446r=0.2652−0.5820mR=0.4164+0.1015m
    TiBP1.95~439r=0.3811−0.9933mR=0.3434+1.4979m
    TnBP1.88~458r=0.2272+0.3410mR=0.5256m0.9292
    TCEP1.91~441r=0.2384–0.5121mR=0.3564−0.5632m
    TCPP2.10~469r=0.3121+1.2603mR=0.2780+1.2912m
    TDCP1.93~449r=0.2008+0.5286mR=0.3215+0.8002m
    TBEP1.92~473r=0.2221+0.9032mR=0.2694+2.2083m
    TPhP1.85~442r=0.1651+0.4826mR=0.3558+0.6809m
    DPEHP1.94~452r=0.2017–0.0458mR=0.2568+3.1222m
    TEHP1.84~467r=0.2052–0.1792mR=0.4434–0.8442m
    TPPO1.80~426r=0.2599–0.0649mR=0.5711+0.4568m
    o-TCP1.94~436r=0.1616+0.5595mR=0.2842+1.8740m
    m-TCP1.94~435r=0.1579+0.5534mR=0.2722+1.2441m
    p-TCP1.88~447r=0.1967+0.3243mR=0.3364+1.4465m
    注:表中m为9家实验室对5个样品测定所得的质量分数平均值。
    下载: 导出CSV

    表  6   方法正确度统计结果

    Table  6   Statistical results of accuracy test for the method.




    Compounds
    推荐值
    Recommended value
    (ng/g)
    最小测量值
    Minimum measurement value
    (ng/g)
    最大测量值
    Maximum measurement value
    (ng/g)
    平均测量值
    Average measurement value
    (ng/g)
    标准偏差SD
    (ng/g)
    相对误差
    RE
    (%)
    TnBP 276±14 267 283 275 4.73 −0.26
    TCEP 925±149 781 1044 910 95.9 −1.66
    TCPP 1200±350 1018 1407 1257 117 4.78
    TPhP 1190±130 837 1228 1126 116 −5.35
    下载: 导出CSV
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出版历程
  • 收稿日期:  2023-05-10
  • 修回日期:  2023-06-05
  • 录用日期:  2023-06-14
  • 网络出版日期:  2023-07-24
  • 刊出日期:  2023-12-30

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