Transcript Document
Measurement and Quality Control of Fatty Acid and trans Fats Determination in Soybeans and Soybean Oil Gina M. Clapper AOCS Technical Services Low Linolenic Acid Soybeans and trans Fatty Acids AOAC International Midwest Section Annual Meeting and Exposition Kansas City, Missouri, USA 7/17/2015 January 1, 2006 all food labels must contain the trans Fatty Acid content if level is at or above 0.5g 7/17/2015 graphic from FDA website Options for the food industry? Keep existing formulations and label appropriately Find alternatives to partially hydrogenated oils PH-Soybean oil is most common 7/17/2015 The Importance of the SQT Initiative Raising the Bar on Beans 7/17/2015 What is SQT? A USB/AOCS collaboration Supports the mission of the checkofffunded Better Bean Initiative (BBI) to accelerate the development and availability of soybean seed with enhanced compositional traits 7/17/2015 Why SQT? Observations Commercial testing labs were using different methods than breeder and seed company laboratories. • NOPA Certified Laboratories use AOCS Methods and analyze > 70% of the referee SBM contracted in the US and use AOCS methods for oilseed analyses • Oilseed Processors predominantly use AOCS methods • Equipment Manufacturers, Seed breeders and Seed Companies generally use internal methods Inability to identify, verify, and quantify enhanced soybean traits limits industry growth in this area Unrealized value and profit from enhanced soybean strains 7/17/2015 Why SQT? (continued) SQT creates and facilitates Systems of verification Reliable analytical results Opportunity for all stakeholders in the soy industry to agree 7/17/2015 SQT Mission To guarantee quality analytical results at all levels in the soybean industry To increase confidence in the ability to identify soybeans with enhanced quality traits To achieve, maintain, and promote peak levels of laboratory accuracy through industry participation in a proficiency program 7/17/2015 Equipment Manufacturers SQT Processors SQT Elevators & Grain Handlers Fats and Oil Professionals Seed Breeders Farmers SQT Referee/Contract Laboratories Seed Companies End User Laboratories SQT Key Concept: Verification Systematic verification of analytical measurements Different sectors create potential for different methodologies Primary methods will be implemented throughout soy continuum First time industry will be standardized 7/17/2015 How do we achieve this? Analyze samples regularly Establish industry-wide acceptance of analytical methods and protocols and their implementation under internationally accepted quality management standards Determine laboratory performance in terms of accuracy and bias 7/17/2015 Key Concept: Certification Certify value-added enhanced soybean varieties for the food and feed industries Identify specific physical traits Validate analytically the presence of these traits Certify the identity of enhanced varieties throughout the continuum 7/17/2015 Advantages of SQT Defines standards for quality assurance Provides quality testing methods Validates industry infrastructure Sets expectations for analytical results Provides traceable standards, reference material, consensus standards 7/17/2015 Advantages of SQT (continued) Promotes and markets testing standards within the industry Increases consumer confidence with system of checks and balances Decreases risk to buyers industry-wide Realizes added value of American enhanced soybeans 7/17/2015 Benefits of SQT Increase the competitiveness of American soybeans in the global marketplace Generate a high level of confidence in enhanced soybean products Better position U.S. soybeans to meet the needs of oil and protein end users and improve the economic value for the U.S. soybean industry 7/17/2015 SQT Phases 2 Secondary Methods Primary Methods 1 Identify Participants & Needs 3 SQT Proficiency Program 4 Laboratory Quality Assurance 5 ISO 17025 Certification 7/17/2015 6 Phase One Identify analysis methods for Protein content Oil content Fatty acid composition analysis (completed) 7/17/2015 Phase Two Develop and validate methods of analysis including the evaluation of secondary methods Library of reference samples to be used for calibrating non-destructive technologies (NIR currently) 7/17/2015 New methods on the horizon Amino Acids Phytate Isoflavones 7/17/2015 Phase Three Identify users and their requirements Seed companies Referee and private laboratories End-user laboratories Elevator and crop handling facilities Establish a core group of expert laboratories 7/17/2015 Phase Four Develop Soybean Quality Traits Laboratory Program, including use of proficiency testing and standards 4 samples 6 times/year Initiated November 2003 7/17/2015 Standards, Methods, and Proficiency Testing Members-only secure access to required methodologies Secure members-only access to Online protocols Secure electronic data reporting forms (can enter moisture, protein, oil and FA profile, report tables) Web- and email-based status, results, proficiency, and rankings reports 7/17/2015 Phase Five Implement laboratory quality assurance Standard methods Certification • Proficiency participation • Results monitoring 7/17/2015 Phase Six Incorporate SQT methods of analysis into ISO 17025 certification and quality audits 7/17/2015 For those who still need to label… 7/17/2015 Evaluation of current testing methods for Linolenic Acid content in soybeans GIPSA (KCMO) evaluated AOCS Official Method Ce 1-62 to determine it was appropriate for determining low-lin oil Internal and commercial laboratories participated in a collaborative study Preliminary results indicate that Ce 1-62 is reasonably accurate, precise and rugged 7/17/2015 Collaborative Study Report Analysis of Fatty Acid Composition PROJECT: Ce-1h-05 The Analysis of Fatty Acid Methyl Esters 7/17/2015 New Method Study: AOCS Official Method Ce 1h-05 Standardization of the current method(AOCS Ce 1f-96): Internal Standard (C21:0) Column type (SP-2560 or CP-Sil 88) Column length (100m) Carrier gas (Hydrogen or Helium) 7/17/2015 following slides borrowed from Dawn McCluckie PARTICIPATION - Samples to 35 labs worldwide - 21 responded, 11 were used TEST MATERIALS - 5 reference samples with labeled chromatograms - 10 randomly coded samples REPORTING - Run in duplicate - Results Area, Area%, TG, and FA - Labeled chromatograms 7/17/2015 Examples of why some participants were eliminated: 1 lab wrong column 1 lab wrong carrier gas 1 lab wrong column length 1 lab only Area % values 7/17/2015 Results- Outliers ODD OUTLIERS REGULAR OUTLIERS Non-reproducible data i.e. not enough responses for statistical analysis, so all reported values considered outliers Analyzable data 7/17/2015 Cochran Single Grubbs Double Grubbs Odd Outlier Example Sample 2 – margarine oil C21:0 internal standard C22:0 C23:0 peak present C24:0 7/17/2015 7/17/2015 Conclusions from this study The peaks are present on the chromatogram The method is good and allows for peak separation Training may be necessary for proper peak identification 7/17/2015 AOCS Official Method Ce 1h-05 Approved by Uniform Methods Committee at the AOCS Annual Meeting Will be available in June with: Labeled chromatograms and reference samples Interactive Excel spreadsheet for calculations Study samples will be released as consensus reference material 7/17/2015 Training AOCS will offer hands-on training workshop for all participants in the collaborative study and methodology meeting AOCS will offer training workshops for the public late summer and into fall to assist industry’s efforts to comply with FDA labeling regulations 7/17/2015 Thank you for your attention! Contact AOCS Technical Services at: [email protected] www.aocs.org/tech 7/17/2015