The Spice Industry
Certified Laboratories is a recognized leader in the areas of spice and seasoning testing. The Laboratory is accredited to ISO 17025 and has an extensive scope for all spice analysis. Our scope of work includes most of the ASTA methods.
As a leader in Food and Drug Administration (FDA Detention without Physical Examination) related testing, our work is accepted by all FDA districts.
The presence of extraneous matter (filth) in spices has long been a major concern of the industry and of FDA. “Filth” can best be described as the extraneous matters left behind by contaminants of the products. These include whole insects, excreta, rodent hairs, and feather barbules. Certified Laboratories stays current with changing FDA methodology and Defect Action Levels (DAL’s), enabling us to tell you quickly and accurately whether or not your shipment will pass the rigid FDA and ASTA standards established for “Filth”.
The ASTA sanitation program also includes testing of oregano for sumac and other adulterants. We are proud to have been part of the working group that established and validated the current method for ASTA.
Light Filth/Microscopic Analysis
With the increased importation of ground spices, and the need to evaluate other commodities for filth, we utilize micro-analytical techniques. By using separation techniques and skilled element identification, a great deal can be discovered about the conditions under which your products were held and produced.
- Acid and Acid-Insoluble Ash
- Cinnamic Aldehyde
- Color (ASTA)
- Crude Fiber
- Heat by HPLC
- Propylene Oxide
- Sieve Analysis
- Steam Volatile Oil (SVO)
- Sudan Dyes
Chemical Residue Testing
Ethylene Oxide (ETO) & Its Byproducts
One approach in use for a considerable length of time, is the treatment of spices with Ethylene Oxide (ETO). As an Epoxide, ETO is fairly reactive. Inevitably there are other reactions involving the epoxide ring, producing a variety of byproducts. Principal among these byproducts is Ethylene Chlorohydrin (ECH) and Ethylene Glycol, both of which are more stable than ETO.
Effective on September 11, 2009, the US tolerance for ETO is 7ppm and for the first time, a tolerance for Ethylene Chlorohydrin has been established at 940 ppm.
Since ETO is fairly volatile and dissipates fairly quickly, the only evidence of exposure to ETO may be the ECH residue. Analytical methods have been designed for this purpose.
The choice of an analytical procedure for ETO and/or its byproducts depends on the purpose for which the results will be used. Clear judgments must be made in advance of testing so as to ensure that the results will be appropriate for their intended use.
For products that actually have been treated with Ethylene Oxide, the ECH levels can be high. Testing on these products is usually done to show compliance with the US tolerance of 940 ppm or the Canadian tolerance of 1500 ppm. The method of choice for this purpose is ASTA (American Spice Trade Association) method 23.3.
If the purpose is to determine if a product has ever been exposed to Ethylene Oxide or contains any component that has been gassed with Ethylene Oxide, the approach is to look for ECH at much lower levels. Testing for these products is usually done to show compliance with the EU tolerance of 20 ppb for ECH. The method we have recently adopted at Certified Laboratories is a mass spectrometric method (Tateo and Bononi, J. Food Comp. and Analysis, V 19, 2006, p 83-87, which satisfactorily covers the lower ranges very successfully.
Determination of ECH levels between 5ppm and 50ppm is a grey area where neither method is suitable. At Certified Laboratories we have addressed this area by modifying the Toteo method by using smaller sample sizes, thus extending the reach of the method upwards. An inevitable concern, of course, is that as sample sizes get smaller, it becomes more difficult to maintain confidence in the representativeness of the sample.
Good communication between the laboratory and the client of the analytical result is essential to ensure that such default choices do not compromise the usability of the analytical result.
To help in deciding which method is most applicable, refer to the table below:
|Analyte||Method||Lowest Level of Detection||Highest Level of Detection||Best Used For|
|ETO||Tateo||10 ppb||2.5 ppm||Compliance with EU/German Requirements|
|ETO||ASTA 23.2||1-5 ppm||1000||Verification of Compliance with US Law|
|ECH||Tateo||20 ppb||10 ppm||Compliance with EU/German Requirements|
|ECH||ASTA 23.3||Approximately 50-100 ppm||>2000 ppm||Verification of Compliance with US and Canadian Rules|
|ECH||Tateo||100-200 ppb||Approximately 50 ppm||Intermediate Levels of ECH|
Please note the above table is also appropriate for Propelyne Oxide Analysis.