FA Distribution in Infant Formula Lipids Analysed by Joint JOCS/AOCS Official Method Ch 3a-19

An international robin round was carried out to validate a method for the quantification of 2-monochloropropane-1,3-diol (2-MCPD), 3-monochloropropane-1,2-diol (3-MCPD) and 2,3-epoxy-1-propanol (Glycidol) being present as fatty acid esters in plant-based food emulsifiers. The evaluated method was a modification of the American Oil Chemist´s Society (AOCS) Official Method Cd29b-13. Briefly, this method consists from parallel analysis of two sample aliquots that are spiked with different sets of internal standards. Mild alkaline interesterification overnight in the freezer releases the core analytes. Reaction stop and glycidol conversion into monobromopropanediol (MBPD) is realised by addition of acidified sodium bromide solution. Subsequently, matrix removal and analyte extraction are achieved by two liquid/liquid (l/l) extraction steps. After derivatisation with phenylboronic acid (PBA) the final extracts are analysed by gas chromatography-mass spectrometry (GC-MS). Quantification is carried out by internal one-point-calibration. 6 laboratories from 4 European countries participated in the trial and reported 8 data sets for 10 test materials (mono- and diacylglycerides as well as polyglycerol polyricinoleates) that were analysed as blind duplicates, giving a total of 20 samples. Result outliers were eliminated according to accepted standards. At 2-MCPD levels above 0.02 mg/kg, 3-MCPD levels above 0.06 mg/kg and glycidol levels above 0.22 mg/kg repeatability (RSDr) ranged from 1.5 % to 24.9 %, reproducibility (RSDR) ranged from 7.8 % to 29.0 % and HORRATR-values ranged from 0.5 to 1.7. The tested method showed to be suitable for the determination of 2-MCPD, 3-MCPD and glycidol in food emulsifiers consisting from mono- and diacylglycerides as well as polyglycerol polyricinoleates.

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Review of Methods for Preparation and Gas Chromatographic Separation of trans and cis Reference Fatty Acids

Journal of AOAC International ◽

10.1093/jaoac/92.5.1310 ◽

2009 ◽

Vol 92 (5) ◽

pp. 1310-1326 ◽

Cited By ~ 42

Author(s):

Pierluigi Delmonte ◽

Ali-Reza Fardin Kia ◽

Qing Hu ◽

Jeanne I Rader

Keyword(s):

Fatty Acid ◽

Reference Materials ◽

Fatty Acid Methyl Esters ◽

Methyl Esters ◽

Fats And Oils ◽

Official Method ◽

Experimental Conditions ◽

Aocs Official ◽

Aocs Official Method ◽

Gas Chromatographic Separation

Abstract In recent years, several countries have implemented new regulations regarding the limitation or labeling of the trans fatty acid (TFA) content of foods and dietary supplements. GC methods for fatty acid (FA) analysis have been updated by improving the separation of TFAs from other FAs, especially trans- and cis-18:1, and by focusing more attention on the FAs contained in fats and oils in lower amounts. FA analysis is affected by the limited availability of reference materials. Identifications are frequently made simply by comparison with separations reported in the literature. This report describes the preparation of mixtures containing fatty acid methyl esters (FAMEs) that are not available as reference materials. These mixtures can be used for FAME identifications. The prepared mixtures are analyzed under the experimental conditions of the American Oil Chemists' Society (AOCS) Official Method Ce 1h-05 and AOCS Recommended Practice Ce 1j-07.

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VALIDASI METODE ANALISIS ASAM LEMAK TRANS DALAM MAKANAN BERDASARKAN AOCS OFFICIAL METHOD Ce 1h-05

Jurnal Teknologi dan Industri Pangan ◽

10.6066/jtip.2016.27.1.40 ◽

2016 ◽

Vol 27 (1) ◽

pp. 40-50

Author(s):

Maria Fransisca Njoman ◽

◽

Nuri Andarwulan ◽

◽

Keyword(s):

Official Method ◽

Aocs Official ◽

Aocs Official Method

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Simultaneous Determination of Free Carnitine and Total Choline by Liquid Chromatography/Mass Spectrometry in Infant Formula and Health-Care Products: Single-Laboratory Validation

Journal of AOAC International ◽

10.1093/jaoac/91.4.777 ◽

2008 ◽

Vol 91 (4) ◽

pp. 777-785 ◽

Cited By ~ 11

Author(s):

Pierre Andrieux ◽

Tamara Kilinc ◽

Christian Perrin ◽

Esther Campos-Giménez

Keyword(s):

Health Care ◽

Standard Deviation ◽

Simultaneous Determination ◽

Relative Standard Deviation ◽

Infant Formula ◽

Free Carnitine ◽

Official Method ◽

Relative Standard ◽

Single Laboratory

Abstract A single-laboratory validation study was conducted for a liquid chromatographic/mass spectrometric (LC/MS) method for the simultaneous determination of the free carnitine and total choline in milk-based infant formula and health-care products. The sample preparation used for both carnitine and choline was adapted from AOAC Official Method 999.14, with an acidic and enzymatic hydrolysis of esterified forms of choline. Carnitine and choline were quantified by ion-pair chromatography with single-quadrupole MS detection, using their respective deuterated internal standards. The repeatability relative standard deviation was 2.5 and 2.1, respectively, for carnitine and choline. The intermediate reproducibility relative standard deviation was <4.7 and 2.4, respectively, for carnitine and choline. The ranges of the average product-specific recoveries were 9298 and 94103, respectively, for carnitine and choline. Choline concentration determined in infant formula reference material SRM 1846 was in agreement with the reference value. The proposed method was compared with the enzymatic methods for a range of products; good correlation (r = 0.99) was obtained, although a significant bias was observed for both analytes. The method, with a short chromatographic run time (7 min), is convenient for routine analysis to enhance analytical throughput and is a good alternative to enzymatic assays.

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Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation: A Multilaboratory Testing Study, Final Action 2011.06

Journal of AOAC International ◽

10.5740/jaoacint.18-0114 ◽

2018 ◽

Vol 101 (6) ◽

pp. 1881-1894 ◽

Cited By ~ 5

Author(s):

Sneh D Bhandari ◽

Ming Gao ◽

John Szpylka ◽

N Collopy ◽

H Chen ◽

...

Keyword(s):

Infant Formula ◽

Collaborative Study ◽

Reference Method ◽

Official Method ◽

Method Performance ◽

Expert Review ◽

Performance Requirements ◽

Relative Standard ◽

Expert Review Panel ◽

Repeatability And Reproducibility

Abstract Background: The need for an updated reference method for folate was identified as a priority by the AOAC’s Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) in 2011. An Expert Review Panel (ERP) found AOAC Official MethodSM 2011.06 suitable for the purpose and approved it as a First Action Official Method. Objective: To determine the repeatability and reproducibility of Method 2011.06: Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation. Methods: A multilaboratory collaborative study was conducted. Eleven laboratories located in five countries participated and completed analysis of all multilaboratory testing (MLT) samples. The study was divided into two parts. In the first part, the laboratories analyzed two practice samples (blindly coded) using the updated folate Method 2011.06. The laboratories providing results within the expected range qualified for part two, in which they analyzed 11 MLT samples in blind duplicates. Results: The results were compared with the Standard Method Performance Requirements (SMPR 2011.006) established for folate. The precision results met the requirements stated in the SMPR for all of the samples. Repeatability and reproducibility relative standard deviations ranged from 3.5 to 6.6 and from 9.0 to 15.7%, respectively. Horwitz ratio values for all of the samples were well below 2 (0.61–1.06). Conclusions: The ERP determined that the method performance met the SMPR requirements in September 2017 after reviewing the presented MLT data. Highlights: The ERP recommended the method for Final Action status.

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