Glycerol Esters of Wood Rosin: 1 Purpose

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
Glycerol Esters of Wood Rosin

https://doi.org/10.1093/9780197610145.003.011
Published: January 2023
Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

AOAC SMPR® 2020.014: Standard Method Performance Requirements
(SMPRs®) for Characterization and Quantitation of Neutral
Components from Glycerol Esters of Wood Rosin (GEWR)
Intended Use: Global Reference Method
1 Purpose
AOAC SMPRs describe the minimum recommended performance characteristics to be used during the
evaluation of a method. The evaluation may be an on-site veri cation, a single-laboratory validation, or a
multi-site collaborative study. SMPRs are drafted by AOAC working groups composed of representatives
from industry, regulatory organizations, contract laboratories, test kit manufacturers, and academic
institutions. Approved by AOAC, AOAC SMPRs may be used for method development, are used by AOAC
expert review panels in their evaluation of validation study data for methods being considered for
SM SM
Performance Tested Methods or AOAC O cial Methods of Analysis , and can be used as acceptance criteria
for veri cation at user laboratories.
2 Applicability
Characterization and quantitation of neutral components of glycerol esters of wood rosin (GEWR) from
Pinus halepensis, Pinus brutia, Pinus palustris, and Pinus elliottii (and potentially other pine species). The most
common analytes are listed in Table 2. The list is not exhaustive and not all compounds on the list may be
present in all GEWR products. All compounds detected above the limit of quantitation (LOQ) must be
identi ed and quantitated.
3 Analytical Technique
A GC method, which could also be performed by GC × GC, that measures the analyte of interest and meets
the following method performance requirements is/are acceptable.
4 Definitions
Limit of quantitation (LOQ).—Lowest level of analyte in a test sample that can be quanti ed at a speci ed
level of precision.
Recovery.—Fraction or percentage of analyte that is measured when the test sample is analyzed using the
entire method.
Repeatability.—Variation arising when all e orts are made to keep conditions constant by using the same
instrument and operator (in the same laboratory) and repeating during a short time period. Expressed as
repeatability standard deviation (SDr); or % repeatability relative standard deviation (%RSDr).
Reproducibility.—Variation arising when identical test materials are analyzed in di erent laboratories by
di erent operators on di erent instruments. The standard deviation or relative standard deviation
calculated from among-laboratory data. Expressed as reproducibility standard deviation (SDR); or %
reproducibility relative standard deviation (%RSDR).
5 Method Performance Requirements

See Table 1.
Table 1 Method performance for neutral components from GEWR
Monoterpene and sesquiterpene neutrals Diterpene and high MW neutrals

a a
LOQ, % 0.005 0.01

a a
Analytical range, % 0.005–1 0.01–1
Recovery, % 80–110 90–107
RSDr, % 6 5.3
RSDR, % 8.8 8
a Percent refers to concentration of a molecule in the GEWR product, e.g., 1% = 0.01 g molecule × per g GEWR.
Table 2 Potential GEWR neutral components from EFSA 2018 opinion

6 System Suitability Tests and/or Analytical Quality Control
(a) Suitable methods will include blanks and appropriate check standards.
(b) Retention time should be stable to ±1%.
(c) Method developer should provide proof of identity and purity of peaks, preferably by MS. NIST Mass
Spectral Library can be helpful.
(d) Method developer should explain how response factors are estimated when a direct standard is not
available.
(e) Purity of the internal standard should be >95%.
7 Validation Guidance
Appendix F: Guidelines for Standard Method Performance Requirements (2019) O cial Methods of Analysis of
AOAC INTERNATIONAL, 21st Ed., AOAC INTERNATIONAL, Rockville, MD, USA
(https://academic.oup.com/aoac-publications)
Validation studies should include at least four GEWR products produced from di erent pine species to
include, but not be limited to, Pinus halepensis, Pinus brutia, Pinus palustris, and Pinus elliottii.
8 Reference Materials
Refer to Annex F: Development and Use of In-House Reference Materials in Appendix F: Guidelines for Standard
Method Performance Requirements (2019) O cial Methods of Analysis of AOAC INTERNATIONAL, 21st Ed., AOAC
INTERNATIONAL, Rockville, MD, USA (https://academic.oup.com/aoac-publications)
9 Maximum Time-to-Results
None.
Developed by AOAC Working Group on Glycerol Esters of Wood Rosins (GEWR). Approved by AOAC GEWR
stakeholders on December 15, 2020.
Posted: February 2021

(SMPRs®) for Characterization and Quantitation of Monoesters from
Glycerol Esters of Wood Rosin (GEWR)
1 Purpose
Performance Tested MethodsSM or AOAC O cial Methods of AnalysisSM, and can be used as acceptance
criteria for veri cation at user laboratories.
2 Applicability
Characterization and quantitation of monoesters of glycerol esters of wood rosin (GEWR) from Pinus
halepensis, Pinus brutia, Pinus palustris, and Pinus elliottii (and potentially other pine species). All compounds
detected above the limit of quantitation (LOQ) must be identi ed and quantitated.
Any analytical technique(s) that measures the analytes of interest and meets the following method
performance requirements is/are acceptable.
4 Definitions
level of precision.
entire method.

See Table 1.
Table 1 Method performance for glycerol monoesters from GEWR
a
Limit of quantitation (LOQ), % 0.5
a
Analytical range, % 0.5–10
Recovery, % 95–105

Repeatability (RSDr), % 3
Reproducibility (RSDR), % 4.4

available.
Appendix F: Guidelines for Standard Method Performance Requirements (2019) 21st Ed., O cial Methods of
Analysis of AOAC INTERNATIONAL, AOAC INTERNATIONAL, Rockville, MD, USA
Method Performance Requirements (2019) 21st Ed., O cial Methods of Analysis of AOAC INTERNATIONAL, AOAC
None.

(SMPRs®) for Characterization and Quantitation of Component
Fractions from Glycerol Esters of Wood Rosin (GEWR)
1 Purpose

expert review panels in their evaluation of validation study data for method being considered for
SM SM
2 Applicability
Characterization and quantitation of component fractions of glycerol esters of wood rosin (GEWR) from
Pinus halepensis, Pinus brutia, Pinus palustris, and Pinus elliottii (and potentially other pine species). The
components of interest include free resin acids, glycerol monoesters, and neutrals. Free resin acids include
all unreacted organic acids present in the GEWR product; glycerol monoesters include all monoesters
present in the GEWR product; and neutrals include all nonsaponi able and nonacidic saponi able
components, mainly monoterpenes, diterpenes, and high-molecular-weight neutrals, in the GEWR
product.
GPC or other analytical technique that measures the components of interest and meets the following
method performance requirements is acceptable.
4 Definitions
level of precision.
entire method.

See Table 1.
Table 1 Method performance for component fractions in GEWR
Free resin acids Monoesters Neutrals

a a a
LOQ, % 0.01 0.5 0.01
a a a
Analytical range, % 0.01–10 0.5%–10 0.01–20
Recovery/accuracy, % 90–107 95–105 90–107
RSDr, % 5.3 3 5.3
RSDR, % 8 4.4 8
a Percent refers to the mass fraction of component in the GEWR product, e.g., 1% = 0.01 g/g.

(c) Method developer should provide proof of identity of peaks.
include, but not be limited to, P. palustris, P. elliottii, P. halpensis, and P. brutia.
None.

(SMPRs®) for Characterization and Quantitation of Residual Resin
Acids from Glycerol Esters of Wood Rosin (GEWR)

1 Purpose
SM SM
2 Applicability
Characterization and quantitation of residual resin acids of glycerol esters of wood rosin (GEWR) from Pinus

halepensis, Pinus brutia, Pinus palustris, and Pinus elliottii (and potentially other pine species). The most
common analytes are listed in Table 1. The list is not exhaustive and not all compounds on the list may be
present in all GEWR products. All residual acids detected above the limit of quantitation (LOQ) must be
identi ed and quantitated.
Any analytical technique that measures the analytes of interest and meets the following method
performance requirements is acceptable.
4 Definitions
Limit of quantitation (LOQ)—Lowest level of analyte in a test sample that can be quanti ed at a speci ed level
of precision.
entire method.

See Table 2.
Table 1 Analytes
Common name PubChem CAS IUPAC name

CID No.
Pimaric 220338 127- (1R,4aR,4bS,7S,10aR)-7-ethenyl-1,4a,7-trimethyl-3,4,4b,5,6,9,10,10a-octahydro-

27-5 2H-phenanthrene-1-carboxylic acid
Isopimaric 442048 5835- (1R,4aR,4bS,7S,10aR)-7-ethenyl-1,4a,7-trimethyl-3,4,4b,5,6,8,10,10a-octahydro-

Levopimaric 221062 79- (1R,4aR,4bS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,9,10,10a-

54-9 octahydrophenanthrene-1-carboxylic acid
Palustric 443613 1945- (1R,4aS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,5,6,9,10,10a-

Abietic acid 10569 514- (1R,4aR,4bR,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-

Dehydroabietic 94391 1740- (1R,4aS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,9,10,10a-

19-8 hexahydrophenanthrene-1-carboxylic acid
Neoabietic 221118 471- (1R,4aR,4bS,10aR)-1,4a-dimethyl-7-propan-2-ylidene-3,4,4b,5,6,9,10,10a-

77-2 octahydro-2H-phenanthrene-1-carboxylic acid
Sandaracopimaric 221580 471- (1R,4aR,4bS,7R,10aR)-7-ethenyl-1,4a,7-trimethyl-3,4,4b,5,6,9,10,10a-octahydro-

Table 2 Method performance for residual acids in GEWR
a
Limit of quantitation (LOQ), % 0.01
a
Analytical range for individual acids, % 0.01–10
Recovery, % 90–107
Repeatability (RSDr), % 5.3
Reproducibility (RSDR), % 8

available.
None.

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

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

Glycerol Esters of Wood Rosin

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

Intended Use: Global Reference Method

5 Method Performance Requirements

Table 1 Method performance for neutral components from GEWR

Monoterpene and sesquiterpene neutrals Diterpene and high MW neutrals

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

Recovery, % 80–110 90–107

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

(b) Retention time should be stable to ±1%.

(e) Purity of the internal standard should be >95%.

Posted: February 2021

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

Intended Use: Global Reference Method

5 Method Performance Requirements

Table 1 Method performance for glycerol monoesters from GEWR

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

Reproducibility (RSDR), % 4.4

6 System Suitability Tests and/or Analytical Quality Control

(b) Retention time should be stable to ±1%.

(e) Purity of the internal standard should be >95%.

Posted: February 2021

Intended Use: Global Reference Method

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

5 Method Performance Requirements

Free resin acids Monoesters Neutrals

Recovery/accuracy, % 90–107 95–105 90–107

RSDr, % 5.3 3 5.3

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

(b) Retention time should be stable to ±1%.

(c) Method developer should provide proof of identity of peaks.

Posted: February 2021

AOAC SMPR® 2020.017: Standard Method Performance Requirements

Intended Use: Global Reference Method

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

5 Method Performance Requirements

Common name PubChem CAS IUPAC name

Pimaric 220338 127- (1R,4aR,4bS,7S,10aR)-7-ethenyl-1,4a,7-trimethyl-3,4,4b,5,6,9,10,10a-octahydro-

Isopimaric 442048 5835- (1R,4aR,4bS,7S,10aR)-7-ethenyl-1,4a,7-trimethyl-3,4,4b,5,6,8,10,10a-octahydro-

Levopimaric 221062 79- (1R,4aR,4bS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,9,10,10a-

Palustric 443613 1945- (1R,4aS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,5,6,9,10,10a-

Abietic acid 10569 514- (1R,4aR,4bR,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

Dehydroabietic 94391 1740- (1R,4aS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,9,10,10a-

Neoabietic 221118 471- (1R,4aR,4bS,10aR)-1,4a-dimethyl-7-propan-2-ylidene-3,4,4b,5,6,9,10,10a-

Sandaracopimaric 221580 471- (1R,4aR,4bS,7R,10aR)-7-ethenyl-1,4a,7-trimethyl-3,4,4b,5,6,9,10,10a-octahydro-

Table 2 Method performance for residual acids in GEWR

Repeatability (RSDr), % 5.3

6 System Suitability Tests and/or Analytical Quality Control

(b) Retention time should be stable to ±1%.

(e) Purity of the internal standard should be >95%.

Posted: February 2021

Downloaded from https://academic.oup.com/aoac-publications/book/45491/chapter/392333544 by guest on 12 March 2023

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