Measurement of methyl mercury (I) and mercury (II) in fish tissues and sediments by HPLC-ICPMS and HPLC-HGAAS

Rajani Jagtap, Frank Krikowa, William Maher, Simon Foster, Michael Ellwood

    Research output: Contribution to journalArticle

    34 Citations (Scopus)

    Abstract

    A procedure for the extraction and determination of methyl mercury and mercury (II) in fish muscle tissues and sediment samples is presented. The procedure involves extraction with 5% (v/v) 2-mercaptoethanol, separation and determination of mercury species by HPLC-ICPMS using a Perkin-Elmer 3 μm C8 (33 mm ÿ 3 mm) column and a mobile phase 3 containing 0.5% (v/v) 2-mercaptoethanol and 5% (v/v) CH3OH (pH 5.5) at a flow rate 1.5 ml min⿿1 and a temperature of 25 °C. Calibration curves for methyl mercury (I) and mercury (II) standards were linear in the range of 0⿿100 μg l⿿1 (r2 = 0.9990 and r2 = 0.9995 respectively). The lowest measurable mercury was 0.4 μg l⿿1 which corresponds to 0.01 μg g⿿1 in fish tissues and sediments. Methyl mercury concentrations measured in biological certified reference materials, NRCC DORM ⿿ 2 Dogfish muscle (4.4 ± 0.8 μg g⿿1), NRCC Dolt ⿿ 3 Dogfish liver (1.55 ± 0.09 μg g⿿1), NIST RM 50 Albacore Tuna (0.89 ± 0.08 μg g⿿1) and IRMM IMEP-20 Tuna fish (3.6 ± 0.6 μg g⿿1) were in agreement with the certified value (4.47 ± 0.32 μg g⿿1, 1.59 ± 0.12 μg g⿿1, 0.87 ± 0.03 μg g⿿1, 4.24 ± 0.27 μg g⿿1 respectively). For the sediment reference material ERM CC 580, a methyl mercury concentration of 0.070 ± 0.002 μg g⿿1 was measured which corresponds to an extraction efficiency of 92 ± 3% of certified values (0.076 ± 0.04 μg g⿿1) but within the range of published values (0.040⿿0.084 μg g⿿1; mean ± s.d.: 0.073 ± 0.05 μg g⿿1, n = 40) for this material. The extraction procedure for the fish tissues was also compared against an enzymatic extraction using Protease type XIV that has been previously published and similar results were obtained. The use of HPLC-HGAAS with a Phenomenox 5 μm Luna C18 (250 mm ÿ 4.6 mm) column and a mobile phase containing 0.06 mol l⿿1 ammonium acetate (Merck Pty Limited, Australia) in 5% (v/v) methanol and 0.1% (w/v) l-cysteine at 25 °C was evaluated as a complementary alternative to HPLC-ICPMS for the measurement of mercury species in fish tissues. The lowest measurable mercury concentration was 2 μg l⿿1 and this corresponds to 0.1 μg g⿿1 in fish tissues. Analysis of enzymatic extracts analysed by HPLC-HGAAS and HPLC-ICPMS gave equivalent results.
    Original languageEnglish
    Pages (from-to)49-55
    Number of pages7
    JournalTalanta
    Volume85
    DOIs
    Publication statusPublished - 2011

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    Mercury
    Fish
    Sediments
    Tissue
    Mercaptoethanol
    Muscle
    Pronase
    Liver
    Cysteine
    Methanol
    Flow rate
    Calibration

    Cite this

    @article{8d8bcd4a7d0444a7a1301ac4343db5ba,
    title = "Measurement of methyl mercury (I) and mercury (II) in fish tissues and sediments by HPLC-ICPMS and HPLC-HGAAS",
    abstract = "A procedure for the extraction and determination of methyl mercury and mercury (II) in fish muscle tissues and sediment samples is presented. The procedure involves extraction with 5{\%} (v/v) 2-mercaptoethanol, separation and determination of mercury species by HPLC-ICPMS using a Perkin-Elmer 3 {\^I}¼m C8 (33 mm {\~A}¿ 3 mm) column and a mobile phase 3 containing 0.5{\%} (v/v) 2-mercaptoethanol and 5{\%} (v/v) CH3OH (pH 5.5) at a flow rate 1.5 ml min{\^a}¿¿1 and a temperature of 25 {\^A}°C. Calibration curves for methyl mercury (I) and mercury (II) standards were linear in the range of 0{\^a}¿¿100 {\^I}¼g l{\^a}¿¿1 (r2 = 0.9990 and r2 = 0.9995 respectively). The lowest measurable mercury was 0.4 {\^I}¼g l{\^a}¿¿1 which corresponds to 0.01 {\^I}¼g g{\^a}¿¿1 in fish tissues and sediments. Methyl mercury concentrations measured in biological certified reference materials, NRCC DORM {\^a}¿¿ 2 Dogfish muscle (4.4 {\^A}± 0.8 {\^I}¼g g{\^a}¿¿1), NRCC Dolt {\^a}¿¿ 3 Dogfish liver (1.55 {\^A}± 0.09 {\^I}¼g g{\^a}¿¿1), NIST RM 50 Albacore Tuna (0.89 {\^A}± 0.08 {\^I}¼g g{\^a}¿¿1) and IRMM IMEP-20 Tuna fish (3.6 {\^A}± 0.6 {\^I}¼g g{\^a}¿¿1) were in agreement with the certified value (4.47 {\^A}± 0.32 {\^I}¼g g{\^a}¿¿1, 1.59 {\^A}± 0.12 {\^I}¼g g{\^a}¿¿1, 0.87 {\^A}± 0.03 {\^I}¼g g{\^a}¿¿1, 4.24 {\^A}± 0.27 {\^I}¼g g{\^a}¿¿1 respectively). For the sediment reference material ERM CC 580, a methyl mercury concentration of 0.070 {\^A}± 0.002 {\^I}¼g g{\^a}¿¿1 was measured which corresponds to an extraction efficiency of 92 {\^A}± 3{\%} of certified values (0.076 {\^A}± 0.04 {\^I}¼g g{\^a}¿¿1) but within the range of published values (0.040{\^a}¿¿0.084 {\^I}¼g g{\^a}¿¿1; mean {\^A}± s.d.: 0.073 {\^A}± 0.05 {\^I}¼g g{\^a}¿¿1, n = 40) for this material. The extraction procedure for the fish tissues was also compared against an enzymatic extraction using Protease type XIV that has been previously published and similar results were obtained. The use of HPLC-HGAAS with a Phenomenox 5 {\^I}¼m Luna C18 (250 mm {\~A}¿ 4.6 mm) column and a mobile phase containing 0.06 mol l{\^a}¿¿1 ammonium acetate (Merck Pty Limited, Australia) in 5{\%} (v/v) methanol and 0.1{\%} (w/v) l-cysteine at 25 {\^A}°C was evaluated as a complementary alternative to HPLC-ICPMS for the measurement of mercury species in fish tissues. The lowest measurable mercury concentration was 2 {\^I}¼g l{\^a}¿¿1 and this corresponds to 0.1 {\^I}¼g g{\^a}¿¿1 in fish tissues. Analysis of enzymatic extracts analysed by HPLC-HGAAS and HPLC-ICPMS gave equivalent results.",
    keywords = "Mercury, Mecaptoethanol extraction, HPLC, ICPMS",
    author = "Rajani Jagtap and Frank Krikowa and William Maher and Simon Foster and Michael Ellwood",
    year = "2011",
    doi = "10.1016/j.talanta.2011.03.022",
    language = "English",
    volume = "85",
    pages = "49--55",
    journal = "Talanta",
    issn = "0039-9140",
    publisher = "Elsevier",

    }

    Measurement of methyl mercury (I) and mercury (II) in fish tissues and sediments by HPLC-ICPMS and HPLC-HGAAS. / Jagtap, Rajani; Krikowa, Frank; Maher, William; Foster, Simon; Ellwood, Michael.

    In: Talanta, Vol. 85, 2011, p. 49-55.

    Research output: Contribution to journalArticle

    TY - JOUR

    T1 - Measurement of methyl mercury (I) and mercury (II) in fish tissues and sediments by HPLC-ICPMS and HPLC-HGAAS

    AU - Jagtap, Rajani

    AU - Krikowa, Frank

    AU - Maher, William

    AU - Foster, Simon

    AU - Ellwood, Michael

    PY - 2011

    Y1 - 2011

    N2 - A procedure for the extraction and determination of methyl mercury and mercury (II) in fish muscle tissues and sediment samples is presented. The procedure involves extraction with 5% (v/v) 2-mercaptoethanol, separation and determination of mercury species by HPLC-ICPMS using a Perkin-Elmer 3 μm C8 (33 mm ÿ 3 mm) column and a mobile phase 3 containing 0.5% (v/v) 2-mercaptoethanol and 5% (v/v) CH3OH (pH 5.5) at a flow rate 1.5 ml min⿿1 and a temperature of 25 °C. Calibration curves for methyl mercury (I) and mercury (II) standards were linear in the range of 0⿿100 μg l⿿1 (r2 = 0.9990 and r2 = 0.9995 respectively). The lowest measurable mercury was 0.4 μg l⿿1 which corresponds to 0.01 μg g⿿1 in fish tissues and sediments. Methyl mercury concentrations measured in biological certified reference materials, NRCC DORM ⿿ 2 Dogfish muscle (4.4 ± 0.8 μg g⿿1), NRCC Dolt ⿿ 3 Dogfish liver (1.55 ± 0.09 μg g⿿1), NIST RM 50 Albacore Tuna (0.89 ± 0.08 μg g⿿1) and IRMM IMEP-20 Tuna fish (3.6 ± 0.6 μg g⿿1) were in agreement with the certified value (4.47 ± 0.32 μg g⿿1, 1.59 ± 0.12 μg g⿿1, 0.87 ± 0.03 μg g⿿1, 4.24 ± 0.27 μg g⿿1 respectively). For the sediment reference material ERM CC 580, a methyl mercury concentration of 0.070 ± 0.002 μg g⿿1 was measured which corresponds to an extraction efficiency of 92 ± 3% of certified values (0.076 ± 0.04 μg g⿿1) but within the range of published values (0.040⿿0.084 μg g⿿1; mean ± s.d.: 0.073 ± 0.05 μg g⿿1, n = 40) for this material. The extraction procedure for the fish tissues was also compared against an enzymatic extraction using Protease type XIV that has been previously published and similar results were obtained. The use of HPLC-HGAAS with a Phenomenox 5 μm Luna C18 (250 mm ÿ 4.6 mm) column and a mobile phase containing 0.06 mol l⿿1 ammonium acetate (Merck Pty Limited, Australia) in 5% (v/v) methanol and 0.1% (w/v) l-cysteine at 25 °C was evaluated as a complementary alternative to HPLC-ICPMS for the measurement of mercury species in fish tissues. The lowest measurable mercury concentration was 2 μg l⿿1 and this corresponds to 0.1 μg g⿿1 in fish tissues. Analysis of enzymatic extracts analysed by HPLC-HGAAS and HPLC-ICPMS gave equivalent results.

    AB - A procedure for the extraction and determination of methyl mercury and mercury (II) in fish muscle tissues and sediment samples is presented. The procedure involves extraction with 5% (v/v) 2-mercaptoethanol, separation and determination of mercury species by HPLC-ICPMS using a Perkin-Elmer 3 μm C8 (33 mm ÿ 3 mm) column and a mobile phase 3 containing 0.5% (v/v) 2-mercaptoethanol and 5% (v/v) CH3OH (pH 5.5) at a flow rate 1.5 ml min⿿1 and a temperature of 25 °C. Calibration curves for methyl mercury (I) and mercury (II) standards were linear in the range of 0⿿100 μg l⿿1 (r2 = 0.9990 and r2 = 0.9995 respectively). The lowest measurable mercury was 0.4 μg l⿿1 which corresponds to 0.01 μg g⿿1 in fish tissues and sediments. Methyl mercury concentrations measured in biological certified reference materials, NRCC DORM ⿿ 2 Dogfish muscle (4.4 ± 0.8 μg g⿿1), NRCC Dolt ⿿ 3 Dogfish liver (1.55 ± 0.09 μg g⿿1), NIST RM 50 Albacore Tuna (0.89 ± 0.08 μg g⿿1) and IRMM IMEP-20 Tuna fish (3.6 ± 0.6 μg g⿿1) were in agreement with the certified value (4.47 ± 0.32 μg g⿿1, 1.59 ± 0.12 μg g⿿1, 0.87 ± 0.03 μg g⿿1, 4.24 ± 0.27 μg g⿿1 respectively). For the sediment reference material ERM CC 580, a methyl mercury concentration of 0.070 ± 0.002 μg g⿿1 was measured which corresponds to an extraction efficiency of 92 ± 3% of certified values (0.076 ± 0.04 μg g⿿1) but within the range of published values (0.040⿿0.084 μg g⿿1; mean ± s.d.: 0.073 ± 0.05 μg g⿿1, n = 40) for this material. The extraction procedure for the fish tissues was also compared against an enzymatic extraction using Protease type XIV that has been previously published and similar results were obtained. The use of HPLC-HGAAS with a Phenomenox 5 μm Luna C18 (250 mm ÿ 4.6 mm) column and a mobile phase containing 0.06 mol l⿿1 ammonium acetate (Merck Pty Limited, Australia) in 5% (v/v) methanol and 0.1% (w/v) l-cysteine at 25 °C was evaluated as a complementary alternative to HPLC-ICPMS for the measurement of mercury species in fish tissues. The lowest measurable mercury concentration was 2 μg l⿿1 and this corresponds to 0.1 μg g⿿1 in fish tissues. Analysis of enzymatic extracts analysed by HPLC-HGAAS and HPLC-ICPMS gave equivalent results.

    KW - Mercury

    KW - Mecaptoethanol extraction

    KW - HPLC

    KW - ICPMS

    U2 - 10.1016/j.talanta.2011.03.022

    DO - 10.1016/j.talanta.2011.03.022

    M3 - Article

    VL - 85

    SP - 49

    EP - 55

    JO - Talanta

    JF - Talanta

    SN - 0039-9140

    ER -