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AOAC Final Action Method 2016.02 (Biotin)
Page 14 of 16
Elution of biotin from IAC:
While assisting a participant investigating low biotin results, it became
apparent that the “back flush” technique was inexactly followed, mainly it seems because the exact
description of this technique was not given. So, rather than performing a true “back flush”, the 3mL
methanol eluate was recycled through the IA cartridge three times. It is possible that this may partly explain
slightly low recovery for some samples, given that the IA cartridge may well have retained a small portion of
this eluent fraction / biotin. The details of the back flush using a syringe plunger / reverse pressure is now
detailed in the method.
Syringe Filter:
At least two laboratories experienced interference with chromatography. The investigation
isolated the issue with syringe filters with extractable chromophores. It was advised to test the filters as part
of the reagent blank preparation
Quality Water:
Quality of water
,
especially the water used for the final extraction is very important to get
clean chromatogram. Type 1 water is recommended and this information will be updated in the method.
UPLC Platform
: The availability of stationary phase (solid-core, kinetex phenyl hexyl) in smaller particle
size for UPLC platforms is encouraging. This would significantly reduce analysis time and improve
throughput, my laboratory is doing further work to validate the change.
Calculation errors:
The calculation error is a common problem which was noticed. It was advised to
participants to use reference samples to prompt any issues with calculation before reporting the results.
REFERENCES
1) Bonjour, J. (1991) Biotin. In: Handbook of Vitamins, L J Machlin Ed, Marcel Dekker, Inc., New York, pp
393- 425
(2) Woollard, D.C., & Indyk, H.E. (2013) Biotin Analysis in Dairy Products. In: B Vitamins and Folates:
Chemistry, Analysis, Function and Effects, Ed V R Preedy, RSC Publishing, Lomdon, UK, pp 377- 395
(3) Livaniou, E., Costopoulou, D., Vassiliadou, I., et al. (2000) Journal of Chromatography A. 881, 331-343
(4) Frappier, F. (1993) Biotin: Properties and Determination in Encyclopedia of food sciences; Food
Technology and Nutrition, Academic Press, London, UK, pp 395-399
(5) Lahely, S., Ndaw, S., Arella, F., et al (1999) Food Chemistry. 65, 253-258
(6) IS EN 15607 (2009) Foodstuffs – Determination of D-biotin by HPLC
(7) Holler, U., Wachter, F., Wehrli, C., et al (2006) Journal of Chromatography B. 831, 8-16
(8) Bitsch, R., Salz, I., & Hotzel, D., (1989) International Journal of Vitamins and Nutritional Research. 59,
59-64
(9) AOAC SPIFAN SMPR 2014.005 (2014)
(10) AOAC Official First Action Method 2016.02
(11) AOAC International, International Study Workbook Version 2.1 for Blind (Unpaired) Replicates
(12) Appendix F: Guidelines for SMPR, AOAC International (2012)
(13) Appendix D: Guidelines for collaborative study procedures to validate characteristics of a method of
analysis, AOAC International (2012).
(14) Biotin (Bio-02) SLV Report 14/05V
ACKNOWLEDGEMENTS
I would like to thank the following individuals for their participation in this study and support during the
course of method set up and the MLT study. Special thanks to Simon Bevis and Elaine Marley of R-
Biopharm Rhône Ltd for supporting the program by providing immunoaffinity columns. Thanks to Neil Choi,
DTS Food Laboratories for analysing the SPIFAN matrices using LCMS/MS method and Shellie Stassie,
Covance Laboratories for organising the MLT samples.
1.
Karen Schimpf and Linda Butler Thompson
, Abbott Laboratories, United States
2.
Isabelle Malaviole
, Aquanal Laboratoire Aquitaine Analyses, France
3.
Michael Hodgson,
George Joseph and Ranjani Devi, AsureQuality Limited, New Zealand
4.
Craig Macfadzean, Xinping Huo and Felicia Lim
, AsureQuality Limited, Singapore
5.
Jirong Wang, Trevor Gill and Lee Kennedy,
DTS Food Laboratories, Australia
6.
Sudhakar Yadlapalli
, FirstSource Laboratory Solutions LLP, India
7.
Harvey Indyk, Brendon Gill, Mumtaz Dole and Cesar Yin
, Fonterra Co-operative, New Zealand
2016.02 (BIOTIN) FINAL ACTION REVIEW
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