SPSFAM Heavy Metals ERP Book

Laboratories that provided feedback: Center for Food Safety and Nutrition Laboratory (FDA)

Kansas City Laboratory (FDA) San Francisco Laboratory (FDA) Southeast Food and Feed Laboratory (FDA) California Department of Public Health, Food and Drug Lab Branch Colorado Dept Public Health Eurofins Central Analytical Laboratories     Florida Department of Agriculture Minnesota Dept of Agriculture New Hampshire Public Health Laboratory State of Nebraska Department of Agriculture FERN Chemical Residue Laboratory The Connecticut Agricultural Experiment Station University of Arizona

Type an X in appropriate column

Statement:

Comments:

Agree Neutral

Disagree

NA

The method, as written, can be followed  properly by someone with intermediate  knowledge of HPLC and ICP‐MS.

XXXXXXXXX XX

X

X

I agree the steps can be followed but I think some type of chart for the  standards would make it more straight forward and easier to calculate.  I  usually spend several hours up front just setting up spreadsheets for the  standards. 

X

The steps of the method are easy to understand. XXXXXXXXX XXX

The method is reliable and consistently provides  results that are accurate and precise. The method produces limited erroneous results  and I do not often rerun samples.

XXXXXXXXX X XXXXXXXXX X XXXXXXXXX X

XX

X

X

XX Agree for juice samples

I have not run this method exactly as written in this version.  We had an  older version of the method that used the hot block.  We no longer have an  HPLC system to use with our ICP‐MS so we haven’t run the method recently.  If not, please list problematic supplies: I have purchased aqueous standards from DMA and MMA from Spex  CertiPrep I’ve had difficulties at times obtaining MMA with < 2% impurities (AsV). I don’t recall having any problems getting standards or reagents.  The  method talks about 1643e but I think the new NIST reference material is  1643f see 4.10.6.  If not, please list problematic equipment:  We no longer have an HPLC system to use with our ICP‐MS so we haven’t  run the method recently.  We had a Waters LC on our Agilent ICP 7500 but  they didn’t interface well together.  We are trying to get an Agilent LC to  run this method.  Analytical column not reliably available, we found,  with significant  backorder delays.  No alternate column found to perform as well.  We try to  keep a backup column on hand for this reason.

The quality control measures are reasonable to  achieve.

X

XX

I can obtain supplies/consumables to perform  the method, if not using the exact materials, I  can locate equivalent materials of the necessary  quality.

XXXXXXXXX XX

XX

I can/did obtain equipment needed to perform  the method, if not using the exact equipment, I  can locate equivalent equipment.

XXXXXXXXX XX

XX

If uses equipment from other vendors, please list manufacturer and model: I have never tried it on another ICP but I know the Waters HPLC worked in  the past although it was difficult to interface in the software.   Perkin Elmer ELAN DRC II with Flexar HPLC

The method performs properly on other  equivalent equipment (difference ICPMS, HPLC,  etc.) from other manufacturers.

XXX

X

XXXXXXXXX

Alcoholic drinks that are particulate‐free.  For example:  hard apple cider, hard pear cider, wine, mead, etc.   Possibly trying out a solid matrix to include the digestion process.   Liquid Dietary Supplement 

Are there any matrices that you would like EAM  4.10 to be used/validated for?

water and water products (flavored water) Other food products such as milk, cheese

 Additional steps for setting up LC and ICPMS; sequence, tuning, data analysis Possibly expanding the quantitation range so dilutions are as crucial. It looks like the method has already been improved by taking away the hot block part of the extraction.   Option to allow labs to oxidize all arsenite to arsenate during dilution if they so choose. Would be nice if labs could choose to  do this with all samples Address any issues seen with AsV interference/ negative peak.  Issue might be limited to our lab?

What would you improve in the method?

Is arsenobetaine necessary, it is expensive

Additional Comments: