AOAC OMB Meeting Book 2-10-16

AOAC OMB Meeting

Example: AOAC Official Method 2015.11 

Chondroitin Sulfate Content in Raw Materials and Dietary Supplements  High‐Performance Liquid Chromatography with Ultraviolet Detection After Enzymatic Hydrolysis 

First Action 2015 

A. Method Performance  The performance criteria in Table 2015.11A is  prescribed by  Standard Methods Performance Requirements  (SMPR)  2014.009 , which was adopted by the AOAC Stakeholder Panel  for Dietary Supplements  (SPDS).  Laboratory(ies)  implementing this method should follow ISO Standard 17025 to verify that the performance of this method in your  laboratory meets the criteria in table 2015.11A.    Please report verification results to AOAC at this link:   AOAC  2015.11 . 

Table 2015.11A: Verification Acceptance Criteria

Analytical Ranges

Parameters 

1‐10% (w/w)

>10‐100% (w/w)

Repeatability (RSD r ) 

≤  3% 

≤2%

Recovery 

92‐105%

98‐102%

B. Materials  Chondroitin sulfate (CS) raw materials from bovine trachea, porcine skin/cartilage, and shark cartilage, and CS  control material from bovine trachea were obtained from Bioiberica (Barcelona, Spain). Dietary supplement  products containing CS (hard‐shell capsules, tablets, chewables, softgels, and liquids) were obtained from  commercial suppliers. Descriptions of the dietary supplement products used in the study are presented in Table  2015.11B .  C. Apparatus  ( a )  LC system .—Beckman 126 dual high pressure mixing pumps (Beckman Coulter, Fullerton, CA, USA), 168 diode  array UV detector, 507e autosampler, and 32 Karat software.  ( b ) Operating conditions .—Mobile phase flow rate, 1.1 mL/min; column temperature, ambient; injection volume,  30 μL; and detection, 240 nm.   ( c )  LC column .—Phenomenex Synergi Polar‐RP, 4.6 × 150 mm, 4 μm particle size (Phenomenex, Torrance, CA, USA).  ( d ) Analytical balance .—Accu‐124 (Fisher Scientific, Pittsburgh, PA, USA), ±0.01 mg readability.  ( e ) Ultrasonic bath .—Model FS60H (Fisher Scientific). 

( f ) pH meter .—Model pH 500 (Oakton, Vernon Hills, IL, USA), ±0.01 pH unit readability.  ( g ) Dry block heater .—Isotemp Dry Bath Incubator (Fisher Scientific), maintained at 37°C.  ( h )  LC injection vials .—2 mL, with caps and Teflon‐coated septa. 

( i )  Limited volume inserts .—200 μL, for LC vials.  ( j )  Syringes .—25, 100, and 500 μL Luer‐Lok. 

D. Reagents  Note : Chemicals from other suppliers meeting the specificationsmay also be used.  ( a )  Solvents .—Acetonitrile, LC grade; water, LC grade; hydrochloric acid, concentrated, ACS reagent grade. 

February 10-11, 2016

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