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液液萃取-固相萃取-气质联用测定指甲中的多溴联苯醚与多氯联苯

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蒙华俊, 陈希超, 蔡凤珊, 庄僖, 郑晶, 张华, 王俊丽. 液液萃取-固相萃取-气质联用测定指甲中的多溴联苯醚与多氯联苯[J]. 环境化学, 2020, (4): 1055-1064. doi: 10.7524/j.issn.0254-6108.2019042505
引用本文: 蒙华俊, 陈希超, 蔡凤珊, 庄僖, 郑晶, 张华, 王俊丽. 液液萃取-固相萃取-气质联用测定指甲中的多溴联苯醚与多氯联苯[J]. 环境化学, 2020, (4): 1055-1064. doi: 10.7524/j.issn.0254-6108.2019042505
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MENG Huajun, CHEN Xichao, CAI Fengshan, ZHUANG Xi, ZHENG Jing, ZHANG Hua, WANG Junli. Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in nails by liquid-liquid extraction, solid phase extraction, and GC-MS[J]. Environmental Chemistry, 2020, (4): 1055-1064. doi: 10.7524/j.issn.0254-6108.2019042505
Citation: MENG Huajun, CHEN Xichao, CAI Fengshan, ZHUANG Xi, ZHENG Jing, ZHANG Hua, WANG Junli. Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in nails by liquid-liquid extraction, solid phase extraction, and GC-MS[J]. Environmental Chemistry, 2020, (4): 1055-1064. doi: 10.7524/j.issn.0254-6108.2019042505
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液液萃取-固相萃取-气质联用测定指甲中的多溴联苯醚与多氯联苯

  • 1. 贵州医科大学公共卫生学院, 贵阳, 550025;

  • 2. 国家环境保护环境污染健康风险评价重点实验室, 生态环境部华南环境科学研究所, 广州, 510655

    • 通讯作者: 王俊丽, E-mail: 411395583@qq.com
  • 基金项目:

    中央级公益性科研院所基本科研业务专项（PM-zx703-201904-122）和广州市科技计划项目（201804010074）资助.

Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in nails by liquid-liquid extraction, solid phase extraction, and GC-MS

  • 1. School of Public Health, Guizhou Medical University, Guiyang, 550025, China;

  • 2. State Environmental Protection Key Laboratory of Environmental Pollution Health Risk Assessment, South China Institute of Environmental Sciences, Ministry of Environmental Protection, Guangzhou, 510655, China

    • Corresponding author: WANG Junli, 411395583@qq.com
  • Fund Project: Supported by the Basic Research Foundation of National Commonwealth Research Institute (PM-zx703-201904-122) and the Guangzhou Science and Technology Program (201804010074).

  • 摘要: 利用液液萃取（LLE）与固相萃取法（SPE）提取和净化人体指甲中的多溴联苯醚（PBDEs）和多氯联苯（PCBs），经浓硫酸除脂后，利用气相色谱-质谱联用仪（GC-MS）测定PBDEs和PCBs.对提取溶剂比例、净化柱类型（复合硅胶柱与固相萃取柱）、固相萃取条件（洗脱溶剂及体积）以及脂肪的去除方法进行了优化，加标回收率较前人基础上均有明显提高.加标回收试验结果显示，PBDEs和PCBs平均基质加标回收率分别为90%—110%和71%—102%，空白加标回收率分别为70%—110%和60%—100%之间，仪器检出限（IDL）分别为0.034—0.120 μg·L-1和0.032—0.392 μg·L-1.本方法快速、简单、高效，能够满足指甲中PBDEs和PCBs的分析.同时本研究利用该方法对电子垃圾拆解地区居民的指甲样品进行测定，PBDEs和PCBs平均浓度分别为623 ng·g-1和148 ng·g-1，BDE（-154、-153、-183、-209）和PCB（-8、-28、-52、-66、-101、-77、-118、-153、-187）在所有样品中均检出，女性指甲中PBDEs与PCBs的浓度普遍高于男性.
    Abstract: Liquid-liquid extraction (LLE) and solid phase extraction (SPE) were used to extract and purify polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in human nails. The extracts were then treated with concentrated sulfuric acid to remove lipid, and the target compounds were analyzed by a gas chromatography tandem mass spectrometry. The extraction solvent ratios, purification methods (composite silica column and SPE column), SPE conditions (elution solvent and volume), and fat removal method were optimized. The recoveries of PBDEs and PCBs in spiked snail samples were 90%—110% and 53%—101%, respectively. Their recoveries in spiked blanks were 70%—110% and 60%—100%, respectively. The instrument detection limits (IDLs) were 0.034—0.120 μg·L-1 for PBDEs and 0.032—0.392 μg·L-1 for PCBs. The developed method was simple, efficient, and timesaving for analyzing nail PBDEs and PCBs. The average total concentrations of PBDEs and PCBs in nail samples of residents near an electronic waste dismantling site were 623 ng·g-1 and 148 ng·g-1, respectively. Four PBDEs (BDE-154, -153, -183, -209) and nine PCB (CB-8, -28, -52, -66, -101, -77, -118, -153, -187) were detected in all the samples. The nail concentrations of PBDEs and PCBs in female were generally higher than those in male.
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  • [1] LIU R, MA S, LI G, et al. Comparing pollution patterns and human exposure to atmospheric PBDEs and PCBs emitted from different e-waste dismantling processes[J]. Journal of Hazardous Materials, 2019, 369:142-149.
    [2] CHAKRABORTY P, ZHANG G, LI J, et al. Seasonal variation of atmospheric organochlorine pesticides and polybrominated diphenyl ethers in Parangipettai, Tamil Nadu, India:Implication for atmospheric transport[J]. Science of the Total Environment, 2019, 649:1653-1660.
    [3] HONG W J, JIA H, DING Y, et al. Polychlorinated biphenyls (PCBs) and halogenated flame retardants (HFRs) in multi-matrices from an electronic waste (e-waste) recycling site in Northern China[J]. Journal of Material Cycles and Waste Management, 2018, 20(1):80-90.
    [4] WANG S, ZHANG S, HUANG H, et al. Characterization of polybrominated diphenyl ethers (PBDEs) and hydroxylated and methoxylated PBDEs in soils and plants from an e-waste area, China[J]. Environmental Pollution, 2014, 184:405-413.
    [5] WANG X T, CHEN L, WANG X K, et al. Occurrence, profiles, and ecological risks of polybrominated diphenyl ethers (PBDEs) in river sediments of Shanghai, China[J]. Chemosphere, 2015, 133:22-30.
    [6] TRINH M M, TSAI C L, CHANG M B. Characterization of polybrominated diphenyl ethers (PBDEs) in various aqueous samples in Taiwan[J]. Science of the Total Environment, 2019, 649:388-395.
    [7] ZHIHUA L, PANTON S, MARSHALL L, et al. Spatial analysis of polybrominated diphenylethers (PBDEs) and polybrominated biphenyls (PBBs) in fish collected from UK and proximate marine waters[J]. Chemosphere, 2018, 195:727-734.
    [8] DIMITRIADOU L, MALARVANNAN G, COVACI A, et al. Levels and profiles of brominated and chlorinated contaminants in human breast milk from Thessaloniki, Greece[J]. Science of the Total Environment, 2016, 539:350-358.
    [9] SHEN H, DING G, HAN G, et al. Distribution of PCDD/Fs, PCBs, PBDEs and organochlorine residues in children's blood from Zhejiang, China[J]. Chemosphere, 2010, 80(2):170-175.
    [10] SCHOETERS G, GOVARTS E, BRUCKERS L, et al. Three cycles of human biomonitoring in Flanders-Time trends observed in the Flemish Environment and Health Study[J]. International Journal of Hygiene and Environmental Health, 2017, 220(2, Part A):36-45.
    [11] HASSINE S B, AMEUR W B, GANDOURA N, et al. Determination of chlorinated pesticides, polychlorinated biphenyls, and polybrominated diphenyl ethers in human milk from Bizerte (Tunisia) in 2010[J]. Chemosphere, 2012, 89(4):369-377.
    [12] SHI J, LV Z, NIE M, et al. Human nail stem cells are retained but hypofunctional during aging[J]. Journal of Molecular Histology, 2018, 49(3):303-316.
    [13] DANIEL C R, PIRACCINI B M, TOSTI A. The nail and hair in forensic science[J]. Journal of the American Academy of Dermatology, 2004, 50(2):258-261.
    [14] SUKUMAR A, SUBRAMANIAN R. Relative element levels in the paired samples of scalp hair and fingernails of patients from New Delhi[J]. Science of the Total Environment, 2007, 372(2):474-479.
    [15] SHI J, LV Z, NIE M, et al. Human nail stem cells are retained but hypofunctional during aging[J]. Journal of Molecular Histology, 2018, 49(3):303-316.
    [16] YAEMSIRI S, HOU N, SLINING M, et al. Growth rate of human fingernails and toenails in healthy American young adults[J]. Journal of the European Academy of Dermatology and Venereology, 2010, 24(4):420-423.
    [17] WANG Y, ZHONG Y, LI J, et al. Occurrence of perfluoroalkyl substances in matched human serum, urine, hair and nail[J]. Journal of Environmental Sciences, 2018, 67:191-197.
    [18] 石莹,张晶,卢丽彬,等.固相萃取-超高效液相色谱-串联质谱法测定人指甲中的三氯生和三氯卡班[J].色谱, 2013, 31(11):1040-1045.

    SHI Y, ZHANG J, LU L B, et al. Determination of triclosan and triclocarban in human nail by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(11):1040-1045(in Chinese).

    [19] WANG Y, SHI Y, VESTERGREN R, et al. Using hair, nail and urine samples for human exposure assessment of legacy and emerging per-and polyfluoroalkyl substances[J]. Science of the Total Environment, 2018, 636:383-391.
    [20] LIU L Y, SALAMOVA A, HE K, et al. Analysis of polybrominated diphenyl ethers and emerging halogenated and organophosphate flame retardants in human hair and nails[J]. Journal of Chromatography A, 2015, 1406:251-257.
    [21] 刘汉霞,张庆华,江桂斌,等.多溴联苯醚及其环境问题[J].化学进展, 2005, 17(3):554-562.

    LIU H X, ZHANG Q H, JIANG G B. Polybrominated diphenyl ethers and their environmental problems[J]. Advances in Chemistry, 2005, 17(3):554-562(in Chinese).

    [22] ZHENG J, CHEN K H, LUO X J, et al. Polybrominated diphenyl ethers (PBDEs) in paired human hair and serum from e-waste recycling workers:Source apportionment of hair PBDEs and relationship between hair and serum[J]. Environmental Science&Technology, 2014, 48(1):791-796.
    [23] PRAGST F, BALIKOVA M A. State of the art in hair analysis for detection of drug and alcohol abuse[J]. Clinica Chimica Acta, 2006, 370(1):17-49.
    [24] JIN J, WANG Y, YANG C, et al. Polybrominated diphenyl ethers in the serum and breast milk of the resident population from production area, China[J]. Environment International, 2009, 35(7):1048-1052.
    [25] LIU L Y, HE K, HITES R A, et al. Hair and nails as noninvasive biomarkers of human exposure to brominated and organophosphate flame retardants[J]. Environmental Science&Technology, 2016, 50(6):3065-3073.
    [26] WIESMVLLER G A, ECKARD R, DOBLER L, et al. The environmental specimen bank for human tissues as part of the german environmental specimen bank[J]. International Journal of Hygiene and Environmental Health, 2007, 210(3):299-305.
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  • 收稿日期:  2019-04-25

液液萃取-固相萃取-气质联用测定指甲中的多溴联苯醚与多氯联苯

    通讯作者: 王俊丽, E-mail: 411395583@qq.com
  • 1. 贵州医科大学公共卫生学院, 贵阳, 550025;
  • 2. 国家环境保护环境污染健康风险评价重点实验室, 生态环境部华南环境科学研究所, 广州, 510655
  • 收稿日期:  2019-04-25
基金项目:

中央级公益性科研院所基本科研业务专项（PM-zx703-201904-122）和广州市科技计划项目（201804010074）资助.

摘要: 利用液液萃取（LLE）与固相萃取法（SPE）提取和净化人体指甲中的多溴联苯醚（PBDEs）和多氯联苯（PCBs），经浓硫酸除脂后，利用气相色谱-质谱联用仪（GC-MS）测定PBDEs和PCBs.对提取溶剂比例、净化柱类型（复合硅胶柱与固相萃取柱）、固相萃取条件（洗脱溶剂及体积）以及脂肪的去除方法进行了优化，加标回收率较前人基础上均有明显提高.加标回收试验结果显示，PBDEs和PCBs平均基质加标回收率分别为90%—110%和71%—102%，空白加标回收率分别为70%—110%和60%—100%之间，仪器检出限（IDL）分别为0.034—0.120 μg·L-1和0.032—0.392 μg·L-1.本方法快速、简单、高效，能够满足指甲中PBDEs和PCBs的分析.同时本研究利用该方法对电子垃圾拆解地区居民的指甲样品进行测定，PBDEs和PCBs平均浓度分别为623 ng·g-1和148 ng·g-1，BDE（-154、-153、-183、-209）和PCB（-8、-28、-52、-66、-101、-77、-118、-153、-187）在所有样品中均检出，女性指甲中PBDEs与PCBs的浓度普遍高于男性.

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