AOAC OMB Meeting Book 2-10-16

AOAC OMB Meeting

Example:     AOAC Official Method 2015.01 

Heavy Metals in Food  Inductively Coupled Plasma–Mass Spectrometry 

First Action 2015 

Note : The following is not intended to be used as a comprehensive training manual. Analytical procedures are  written based on the assumption that they will be performed by technicians who are formally trained in at least  the basic principles of chemical analysis and in the use of the subject technology.  {Applicable for the determination of heavy metals [arsenic (As), CAS No. 7440‐38‐2; cadmium (Cd), CAS No. 7440‐ 43‐9; lead (Pb), CAS No. 7439‐92‐1; and mercury (Hg), CAS No. 7439‐97‐6] at trace levels in food and beverage  samples, including solid chocolate, fruit juice, fish, infant formula, and rice, using microwave digestion and  inductively coupled plasma–mass spectrometry (ICP‐MS).}  Caution : Nitric acid and hydrochloric acid are corrosive. When working with these acids, wear adequate protective  gear, including eye protection, gloves with the appropriate resistance, and a laboratory coat. Use an adequate  fume hood for all acids. Hydrogen peroxide is a strong oxidizer and can react violently with organic material to give  off oxygen gas and heat. Adequate protective gear should be worn. Many of the chemicals have toxicities that are  not well established and must be handled with care. For all known chemicals used, consult the Material Safety  Data Sheet (MSDS) in advance.  Etc., etc., etc.  A. Method Performance  The performance criteria in Table 2015.01A is  prescribed by  Standard Methods Performance Requirements  (SMPR)  2012.00 7 , 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  2015.01 . 

Table 2015.01A Verification Acceptance Criteria  Limit of Quantitation (LOQ) 

Parameters 

Ranges 

Repeatability (RSD r ) 

Recovery 

≥ 10 ppb to 100 ppb 

≤ 15% 

60% ‐ 115% 

>100 ppb to 1 ppm 

 ≤ 11% 

80% ‐ 115% 

> 1 ppm to 10 ppm 

≤ 7.3% 

80% ‐ 115% 

B. Principle  Food samples are thoroughly homogenized and then prepared by microwave digestion and the addition of dilute  solutions of gold (Au) and lutetium (Lu). The Au is used to stabilize the Hg in the preparation, and the Lu is used to 

February 10-11, 2016

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