Scribd Logo
Upload

Welcome to Scribd!

  • Faqs On Honey Testing Methods For Detecting Adulteration With Sugar Syrups

    Uploaded by

    Hallo Sunshine
    11 views4 pages
    1) There are multiple methods used to detect honey adulteration with sugar syrups, including 13C isotope ratio testing, NMR profiling, and LC-HRMS. Each method has strengths and weaknesses. 2) When used together, these methods provide the most reliable detection of adulteration, as 13C isotope can detect some C4 sugars, NMR profiling checks for known and unknown syrups, and LC-HRMS has very high sensitivity in detecting markers from sugar syrups. 3) No single test can detect all types of adulteration on its own. The best approach is to use all three methods combined to leverage their individual strengths and more comprehensively test honey authenticity.

    Original Description:

    Original Title

    NHB-Honey-Testing-FAQs

    Copyright

    © © All Rights Reserved

    Available Formats

    PDF, TXT or read online from Scribd

    Did you find this document useful?

    Is this content inappropriate?

    Report this Document
    1) There are multiple methods used to detect honey adulteration with sugar syrups, including 13C isotope ratio testing, NMR profiling, and LC-HRMS. Each method has strengths and weaknesses. 2) When used together, these methods provide the most reliable detection of adulteration, as 13C isotope can detect some C4 sugars, NMR profiling checks for known and unknown syrups, and LC-HRMS has very high sensitivity in detecting markers from sugar syrups. 3) No single test can detect all types of adulteration on its own. The best approach is to use all three methods combined to leverage their individual strengths and more comprehensively test honey authenticity.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Flag for inappropriate content
    Download as pdf or txt
    11 views4 pages

    Faqs On Honey Testing Methods For Detecting Adulteration With Sugar Syrups

    Uploaded by

    Hallo Sunshine
    1) There are multiple methods used to detect honey adulteration with sugar syrups, including 13C isotope ratio testing, NMR profiling, and LC-HRMS. Each method has strengths and weaknesses. 2) When used together, these methods provide the most reliable detection of adulteration, as 13C isotope can detect some C4 sugars, NMR profiling checks for known and unknown syrups, and LC-HRMS has very high sensitivity in detecting markers from sugar syrups. 3) No single test can detect all types of adulteration on its own. The best approach is to use all three methods combined to leverage their individual strengths and more comprehensively test honey authenticity.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Flag for inappropriate content
    Download as pdf or txt
    of 4

    FAQS ON HONEY TESTING METHODS FOR

    DETECTING ADULTERATION WITH SUGAR SYRUPS

    WHAT TESTING METHODS ARE


    USED TO DETECT HONEY ADULTERATION?

    Ensuring honey authenticity is one of the great challenges facing the honey industry today. Over the past
    half century, a number of honey testing methods have been developed to detect food fraud. To date, there is
    no single universal analytical method available which is capable of detecting all types of adulteration with
    adequate sensitivity. A variety of methods are used to detect honey adulteration, each test has strengths and
    weaknesses; when used in combination these tests offer the most reliable predictor of honey’s purity from sugar
    syrup adulteration .

    1. 13
    C Stable Carbon Isotope Ratio Method (SCIRA) or EA/IRMS.
    Limit of C4 Syrup Detection 7%
    Originally developed in the 1970’s and the only AOAC Official method – 998.12 C4 Plant Sugars in Honey.
    This method can detect only corn or sugar cane derived syrups (C4 sugars), it cannot detect syrups made
    from beets, rice, wheat or other plants (C3 sugars).

    2. C Stable Carbon Isotope Ratio Method paired with a Liquid Chromatograph or EA/LC-IRMS.
    13

    Limit of Syrup Detection 3-5% C4, 10-30%* C3


    Developed in 2008, this method is also good for directly determining adulteration with C4 sugar syrups;
    but can also indirectly detect adulteration with C3 sugar syrups, though with less sensitivity than for C4.
    *(some custom C3 syrups are undetectable by this method).

    3. Nuclear Magnetic Resonance Profiling or NMR.


    Limit of Syrup Detection 10-40%
    This is a rapid screening method designed to test for both known and unknown syrups, as well as to
    detect prohibited processing methods and other potential manipulations of pure honey. NMR compares
    each sample against a database of curated pure honey samples using an array of 53 parameters to
    detect sugar syrups and a quantitative analysis of 36 compounds. This technique is not as sensitive as
    other methods, but can also be used to determine the country of origin and botanical source of honey.

    4. Liquid Chromatography-High Resolution Mass Spectrometry analysis or HRMS.


    Limit of Syrup Detection as low as 5%
    Similar to NMR, this method can test for both known and unknown syrups in honey, although in the case
    of HRMS the focus is on the identification of specific markers typical of sugar syrups. HRMS is highly
    sensitive, detecting very low concentrations of telltale syrup markers where they may be present in
    otherwise pure honey.

    FAQs on Honey Testing Methods for Detecting Adulteration with Sugar Syrups 1
    WHAT ARE THE DIFFERENCES
    BETWEEN THESE TESTS?

    13C EA/LC-IRMS (C3/C4 sugar detection)


    This test was developed and validated in 2004-2007 to detect the presence of added sugars both from C4
    plants (e.g. corn and cane syrup) and C3 plants (e.g. rice, wheat, beet syrup). It has been used commercially for
    honey adulteration analysis since 2007. The first ISO 17025 accreditation was achieved in 2008.
    • This method differs from the AOAC SCIRA method in that it makes use of a liquid chromatograph to
    separate each major sugar and evaluate individually. This improves the sensitivity and makes possible the
    detection of some C3 sugars.
    • In 2015-2017, this method was used in an EU Commission monitoring program to check honey products for
    adulteration on the European market (~2300 samples, ~14% non-compliance).
    • Limit of Detection for C4 sugars: 3-5 % (depending on honey type and adulterant)
    o C4 sugars > 7% can be quantified by this method.
    • Limit of Detection for C3 sugars: 10-30 % (depending on honey type and adulterant)
    o C3 sugars percentage cannot be quantified by this method and some are undetectable.
    • Note: This method cannot detect the tailor-made syrups which are adapted to the honey type or a host
    of other illegal processing methods.

    NMR Profiling
    NMR is short for nuclear magnetic resonance. NMR-spectroscopy has been used since the 1970s for
    quantification and structural analysis and is becoming a reliable method to officially test the authenticity of
    food (e.g. fruit juice, wine, edible oils, and honey).
    • Research and Development for the application of NMR to honey began in the late 1990s, and was
    introduced for routine analysis (honey profiling) in 2013.
    • NMR compares the spectra of commercial honeys with a reference database of authentic honeys. At
    present, there are several reference databases. The most well-known are owned and maintained by
    Bruker and Eurofins.
    • No harmonized and publicly available reference database exists for NMR at this time. (under discussion
    at the EU Joint Research Centre)
    • New additions to existing databases can result in changes to interpretations of spectra and the
    determination of sample purity.
    • Each NMR lab must use the same analytical procedure, instrumentation and reference database to
    achieve identical results (e.g. the Bruker Honey Screener). If different NMR methodologies and databases
    are used, cross-check benchmarking is necessary to achieve comparable result interpretations. Status
    quo: >98% agreement between the main commercial databases (Bruker, Eurofins).
    • Most applicable for verifying the authenticity of honeys that have known, singular botanical and
    geographical origin; in the case of blends of different botanical and geographical origins, only the purity
    of honey can be checked.

    FAQs on Honey Testing Methods for Detecting Adulteration with Sugar Syrups 2
    NMR Profiling (continued)
    • Subjective “expert interpretation” is often utilized to conclude a sample is adulterated, even when the
    honey is determined to be acceptable by comparison to the database alone.
    • Not the most sensitive method for detection of honey dilution with syrups (LOD 10-15% in the best case
    and as high as 40% with tailored syrups), but well suited to general screening for adulteration, botanical/
    geographical origin verification and detection of illegal processing practices (e.g. resin technology).
    • May give false positive results for unique honeys not yet included in the database (a false positive is the
    finding that a pure honey appears adulterated according to the database).
    • Once measured, data for each sample is retained and can be compared against future additions to the
    syrup database without re-processing the original sample.

    Liquid Chromatography-High Resolution Mass Spectrometry (LC-HRMS)


    LC-HRMS is the most recently developed method and is not yet in widespread use. There are two approaches
    to the application of the method, one uses a stand-alone HRMS instrument and the second uses a paired
    approach with HRMS to identify new markers and LC-MS/MS to process routine samples once markers are
    identified.
    • HRMS first became viable with the development of highly sensitive and affordable instruments in 2015.
    • Does not require an extensive reference database of authentic honeys for foreign sugar detection, but
    uses targeted screening for adulterant trace marker compounds intrinsic to sugar syrups (exact mass
    determination, publicly available databases).
    • The method uses a screening approach to identify syrup-specific target compounds in a sample. This
    approach will confirm the presence of known compounds and identify any new or unusual compounds
    foreign to honey and suspect as indicators of sugar syrup. More than 15,000 compounds can be
    simultaneously screened.
    • Once LC-HRMS has identified known adulterants (>400 known adulterant markers identified to date),
    future analysis can be done using another instrument; LC-MS/MS. Each syrup has characteristic multi-
    marker profiles allowing for an identification with a high confidence level. LC-MS/MS is not well suited
    to screening for new or unusual compounds but is very capable of targeting those first identified using
    HRMS.
    • HRMS methods offer excellent sensitivity for adulteration markers (better than IRMS and NMR), but it is
    not capable of accurately quantifying the level of sugar syrup addition, nor the exact source of the syrup
    addition. For the method to successfully quantify the amount of added sugar it is necessary to have a
    sample of the syrup used to adulterate the honey which is not usually the case.
    • HRMS replaces older single-marker methods such as:
    o SM-B (beet syrup)
    o SM-R/TM-R (rice syrup)
    o E150d (caramel color)
    o Oligosaccharides (syrups produced from starch)
    o Mannose/Psicose: tailor-made and refined syrups
    • Once measured, data for each sample is retained and can be compared against future additions to the
    syrup database without re-processing the original sample.

    FAQs on Honey Testing Methods for Detecting Adulteration with Sugar Syrups 3
    WHAT TEST IS BEST FOR
    DETECTING HONEY ADULTERATION?

    The current best recommendation is to apply all three methods in combination in order to leverage the
    inherent strengths of each.

    Strengths and Weaknesses of each Testing Method

    13C EA/ LC- NMR-


    Determination Of LC-IRMS HRMS Profiling

    C4 Sugar n n n n Very Effective in Detecting


    n Somewhat Effective in Detecting
    C3 Sugar n n n
    n Not Effective in Detecting
    Tailor-made syrups n n n
    Illegal (Resin) Processing n n n
    Moisture Reduction n n n
    Botanical and
    Geographical Origin
    n n n

    The National Honey Board is committed to supporting the development and refinement of all honey testing
    methods as we work towards the common goal of eliminating food fraud in our industry. If you have any
    additional questions, please email or call the National Honey Board.

    call 303-776-2337 email [email protected]

    FAQs on Honey Testing Methods for Detecting Adulteration with Sugar Syrups 4

    You might also like