Eurofins Supplement Analysis Center Bailey Ireland, Hong You, Ph.D - - PowerPoint PPT Presentation

Eurofins Supplement Analysis Center

Bailey Ireland, Hong You, Ph.D

1997 2002 2005 2015 2017 Start Up

Eurofins Start up lab with 10 staff for SNIF- NMR 1 Country 1 Lab

1982

Alpha labs founded Eurofins Founded

2001 Expansion

Expansion thru IPO in Paris. 10 Countries 50 Labs

1987 1999

Eurofins Acquisition

2010

ISO 17025

2004 Infrastructure

Investment in Infrastructure 15 Countries 100 Labs

Today

Globally recognized testing leader 39 Countries 400 Labs

Global Growth

Growth thru Acquisitions and New Labs 30 Countries 150 Labs

Infrastructure

Building purchase and lab expansion

Company History

Celebrating 30 Years 1996

Relocation to Redwood Way Rebranding to Eurofins Supplement Analysis Center

FDA Requirements

Dietary Supplement Supplier/Manufacturing

• Responsible for making sure their products are safe

BEFORE they go to the market

• Follow current Good Manufacturing Practice
• Notify FDA of new ingredients
• Report adverse events

• Caffeine Reference Material to ISO

17034 Certified Reference Material

Case Study

#1 - Upgrade

• Caffeine

– Upgraded RM – Reagent grade RM to CRM – Potential for higher quality RM

• Improved measuring equipment and techniques
• Reference Material Providers issue more information

Case Study

#1 - Upgrade

• Caffeine

– Upgraded RM – Reagent grade RM to CRM – Potential for higher quality RM

• Improved measuring equipment and techniques
• Reference Material Providers issue more information

Case Study

#1 - Upgrade

Case Study #1 - Upgrade

• Reference Material

– General Term – Can by quantitative or qualitative

Case Study #1 - Upgrade

• Certified Reference Material

– Characterized by valid procedures – Reference material certificate: specified properties, uncertainty, traceability – Relevant uncertainties reported

• Hesperidin In-House Reference

Material

Case Study

#2 – Checks and Balances

Case Study #2 – Checks and Balances

Bioflavonoids - HPLC-UV

• Control Reference Material

– Selection – Preparation

• Issue: Hesperidin control

results failing low

Case Study #2 – Checks and Balances

RM Calculation Mode

• Purity % calculated as HPLC Area %
• Purity % calculated as HPLC %
• HPLC % calculated based on calibration curve
• RM inflated results in control chart
• New control chart created with CRM
• Consider RM quality and assay method

• Troxerutin Investigation

Case Study

#3 – Reliable Sources

Case Study #3 – Reliable Sources

Troxerutin

• High result bias in sample
• Out of Specification (OOS) investigation

– RM had high purity and low moisture content compared to other RM – Contacted Supplier

• Samples re-tested before reporting
• Vendor Evaluation for All Suppliers

Vendor Evaluation

• Quality Assurance

– ISO Certification

• Support

– Expiration Dates – Certificate of Analysis – Assay Method – Phone and onsite support

Case Study

#3 – Reliable Sources

Master sample workflow tool

eLIMS

Customer complaint and Investigation System

eJIRA

Global test catalog

ComLIMS

Electronic document management System

Updated D4

Internal log tracking and alert system

SharePoint

Document and Report Systems

Documentation

• Storage information located on

Certificate of Analysis

• Label lab performance/R&D RM
• Organize by assay method/use

– Subcategories: Chemical name, Method, Method Test Family

Organizing and Storing RM

• B12 Method Development

Case Study

#4 – R&D

Case Study #4 – R&D

Vitamin B12

• Method Development
• Issue: Co-eluting peaks
• Analyte Identification

– RT – Spectrum

Case Study #4 – R&D

Optimization of HPLC condition – standard mixture Seems to be the best…

Methylcobalamine Water extraction Phosphate buffer extraction Methylcobalamine

*

* *

Reduce flow rate for better separation

* *

• Hyaluronic Acid Method Validation

Case Study

#5 – Solubility

Case Study #5 – Reliable Sources

Hyaluronic Acid-CE

• Solubility Difference:

– Hyaluronic acid sodium salt from rooster comb – Hyaluronic acid sodium salt from Streptococcus equi

• Method validated RM
• RM Changes – equivalent RM need to be evaluated

• Ginger Label Claim Recovery

Case Study

#6 – Calibration

Case Study #6 – Calibration

Ginger-HPLC-UV

• 3 of 12 samples OOS

– Capsaicin response factor – Each analyte calibrated

ID code Matrixces Sample form Estimated level Repeatability test result Recovery Claim met? 251 Rhizome powder Raw material 1% Total nonvolatile ginger constituents* 1.10% 110% Yes 099 Rhizome dry extract Raw material 5% Total nonvolatile ginger constituents 5.18% 104% Yes 875 Tablet Finished product 0.3% Total nonvolatile ginger constituents* 0.05% 17% No 063 Tablet Finished product 0.03% Total nonvolatile ginger constituents* 0.03% 100% Yes 580 Capsule Finished product 2.51% total nonvolatile ginger constituents 3.08% 123% Yes 101 Liquid Capsule Finished product 0.58% zingerone 0.50% zingerone 86% No 986 Rhizome oleoresin - supercritical CO2 extract Raw material 50% Total nonvolatile ginger constituents 40.2% 80% No 648 Lean muscle recovery supplement powder Finished product 0.01% 6-Paradol 0.01% 6- Paradol 100% Yes 420 Tincture Finished product Unknown 0.45% N/A N/A 889 Softgel capsules Finished product 5.10% Total nonvolatile Ginger constituents 5.47% 107% Yes 740 Rhizome powder Raw material 1% Total nonvolatile ginger constituents* 0.80% 80% No 692 Rhizome dry extract Raw material Unknown 3.64% N/A N/A * Estimated assuming ginger rhizome powder contains 1% total nonvolatile ginger constituents and ginger dry extract contains

Conclusion

• Improving Reference Materials Quality
• Quality Control
• Correct RM Storage and Organization
• Use RM to Identify
• Source of RM Matters
• Quantification Method