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    Stakeholder Panel On Endocrine Disruptors: 1 Applicability

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    Stakeholder Panel On Endocrine Disruptors: 1 Applicability

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    392328693

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    13 views2 pages

    Stakeholder Panel On Endocrine Disruptors: 1 Applicability

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    ruben castro

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    of 2

    O icial Methods of Analysis of AOAC INTERNATIONAL 22nd Edition (22)

    Dr. George W Latimer, Jr. (ed.)

    https://doi.org/10.1093/9780197610145.001.0001
    Published: 2023 Online ISBN: 9780197610145 Print ISBN: 9780197610138

    CHAPTER

    Stakeholder Panel on Endocrine Disruptors


    https://doi.org/10.1093/9780197610145.003.004
    Published: January 2023

    Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392328693 by guest on 12 March 2023


    AOAC SMPR® 2010.007: Standard Method Performance Requirements
    (SMPRs®) for Quantitative Determination of Estrone (E1) in Freshwater

    Intended Use: Quantitative Measurement by Trained Personnel

    1 Applicability
    Rapid screening-level determination of dissolved estrone at environmental levels in freshwater containing
    up to 1000 mg/L (ppm) of total suspended solids (TSS) and 1000 mg/L (ppm) of dissolved organic carbon
    (DOC). Estrone is also known as E1; oestrone; or 3-hydroxy-13-methyl-6,7,8,9,11,12,13,14,15,16-
    decahydrocyclopenta[a]phenanthren-17-one. CAS No.: 53-16-7.

    2 Analytical Technique
    Any analytical technique that meets the following method performance requirements is acceptable.

    3 Definitions
    Freshwater.—Naturally occurring water on the Earth’s surface in wetlands, ponds, lakes, rivers,streams, and
    aquifers exclusive of brines, seawater, and brackish water. (USGS de nition: Less than 1000 mg/LTSS.)

    DOC.—The fraction of total organic carbon (all carbon atoms covalently bonded in organic molecules) in
    water that passes through a 0.45 micron pore-diameter lter.

    Limit of detection (LOD).—Equivalent to the term “Method Detection Limit” (MDL) used by the U.S.
    Environmental Protection Agency: The minimum concentration of a substance that can be measured and
    reported with 99% con dence that the analyte concentration is greater than zero, and is determined from
    analysis of a sample in a given matrix containing the analyte.

    Limit of quanti cation (LOQ).—The level above which quantitative results may be obtained with a speci ed
    degree of con dence.

    Precision (repeatability).—Variation arising when all e orts are made to keep conditions constant by using
    the same instrument and operator, and repeating during a short time period. Expressed as the % standard
    deviation (SD); or % relative standard deviation (%RSD).

    Recovery factor.—The ratio of the observed mean test result to the true value. Recovery % = [meanobs/true] ×
    100.

    Reproducibility.—RSD calculated from among-laboratory data.

    4 Method Performance Requirements


    See Table 1.
    5 System Suitability Tests and/or Analytical Quality Control
    Suitable methods will include blank check samples and check standards at the lowest point and midrange
    point of the applicability range.

    If a candidate method is a commercially provided method, then the method provider must provide
    documentation in the validation package to demonstrate (1) suitable lot-to-lot consistency, and (2) stability
    over the claimed shelf-life of the reagents.

    6 Reference Method(s)
    No reference method exists. (EPA 1698 could be used. GC-HRMS-MS could be used as an instrumental
    method with suitable sensitivity.)

    7 Reference Material(s)

    Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392328693 by guest on 12 March 2023


    None available.

    8 Validation Guidance
    Preservation of prepared samples must be considered and consistent among laboratories participating in a
    validation.

    Study materials should be analyzed by tandem mass spectrometry.

    SM
    Recommended level of validation: O cial Methods of Analysis .

    9 Maximum Time-to-Signal
    No maximum time.

    Approved by AOAC Stakeholder Panel on Endocrine Disruptors on September 20, 2010.

    Table 1 Method performance requirements

    Analytical range 2–200 ng/L (ppt)

    LOD 0.5 ng/L (ppt)

    LOQ ≤2 ng/L (ppt)

    Precision (repeatability; RSDr) 2 ng/L (ppt) ≤110%

    20 ng/L (ppt) ≤50%

    200 ng/L (ppt) ≤30%

    Recovery factor 50 to 120% of mean spiked recovery over the range of the assay

    Reproducibility (RSDR) 2 ng/L (ppt) ≤165%

    20 ng/L (ppt) ≤75%

    200 ng/L (ppt) ≤45%

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