Melamine Testing

Monday, February 16, 2009

Melamine Testing

In the spring of 2007 several dogs and cats died in North America due to the adulteration of wheat gluten with melamine, the basic ingredient in melamine resins. The pets died due to damage from crystals formed in their kidneys by the combination of melamine and its metabolite cyanuric acids. A year and a half later, adulteration of milk products with melamine in China led to one of the biggest food scandals of the last decades. This led to kidney problems in thousands of babies and infants and in some cases even resulted in deaths.

Currently, contaminated candy and cookies from East Asia are being exported and have been found in the EU. Accordingly, the EU has imposed an import ban on all baby and infant food from China and requires the analysis of melamine on all imported food containing either more than 15 % or an unknown amount of milk or milk powder. The maximum allowed limit is 2.5 mg / kg.

In response to the melamine crisis, Eurofins Central Analytical Laboratories offers advanced melamine testing services. The established methods utilized are based on US Food and Drug Administration’s GC-MS and LC-MSMS methods.

Due to high equipment capacities, Eurofins laboratories are now able to analyze globally over 250 samples per day. The standard turn-around-time is 5 to 7 days. Express analysis is also available with reports issued within 24 to 36 hours of receipt of sample.

FDA Import Alerts

Eurofins CAL has the most appropriate testing strategies and sampling services for FDA Detention Import Alerts #99-30 and #99-31. We can provide a complete testing solution for the importer, including sampling, testing , FDA submittal package and consulting on FDA intervention issues.

Analytes

The following compounds are among those covered by the current FDA GC-MS method:

Melamine
Cyanuric Acid
Ammeline
Ammelide

Test Method

FDA method LIB 4421 by LC-MSMS: This method is best used for milk, infant formula, and samples containing milk products. This method includes, Melamine, Cyanuric Acid, Ammeline, and Ammelide. Our present Limit of Quantification (LOQ) for melamine is 0.25 ppm. The turnaround is 5 to 10 working days. We offer a rush option of 3 working day turnaround time. The rush option includes a 50% up charge.

FDA method LIB 4422 by LC-MSMS: This method can achieve an LOQ as low as 0.05 ppm for melamine in dry products and 0.01 ppm in fish. The turnaround is 5 to 10 working days. This method is recommended to meet international regulations that require the lowest possible detection limits. We offer a rush option of 3 working day turnaround time. The rush option includes a 50% up charge.

FDA GC-MS method 2.1: This method is best used for pet food, and most feed ingredients. The turn around is 5 to 7 working days. We can expedite the turn around to 2 to 3 working days at a 50 % up charge. Our present Limit of Quantification (LOQ) is 10 ppm.

The method of choice will have to be determined depending on each individual sample type and importing or exporting circumstances. The GC-MS method has a good response on most feeds, soy products, protein isolates, wheat glutens, etc..The LC-MSMS method is used for infant formula, milk powder, most preservatives, vitamins, fertilizers, amino acids, etc.

Quality Assurance

Method cross validated within multiple Eurofins laboratories worldwide
Use of a methylated melamine compound as an internal standard
Recovery of the internal standard is monitored
Use of blanks, and spikes for each sample type within an analytical batch
Continuing calibration verification every 15 samples

References

FDA published method for Melamine and related analogs.