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Analytical / Chromatography > Food Safety > Adulterants & Additives
Food Safety

Adulterants & Additives

Melamine
Diethylene Glycol (DEG)
Malachite Green Dye
Antimicrobial Agents - Chloramphenicol, Fluoroquinolones


Melamine back to top

Nutrition labeling requirements require disclosure of food product ingredients and their associated nutritional value to ensure food quality. Recently, infant formula (milk-based products) and dog food ingredients (wheat gluten binders) supplied from China were chemically modified with melamine, a nitrogen-based compound, to falsely boost the reported protein levels. Proteins are typically the only sources of nitrogen in food, and in most test methods the relative protein concentration is estimated from the amount of detected nitrogen. As a result of melamine adulteration, thousands of pets became sick and many died; a couple of hundred thousand children became sick with kidney ailments, and a handful of deaths resulted. The toxicity of melamine results from the formation of insoluble crystals of melamine and cyanuric acid (a by-product of melamine); these crystals cause the formation of kidney stones in pets and babies. Besides melamine and cyanuric acid, two other melamine-related compounds, ammeline and ammelide, were found in adulterated pet food and are now included in regulatory test methods. The MRL for melamine is listed below and is accepted by food safety agencies around the world.

Maximum Residue Limit (MRL) for Melamine: 1 mg/kg and 2.5 mg/kg in baby formula and milk products


Applications
Discovery SCX SPE columns and Ascentis Express HILIC HPLC columns are effective tools for extraction and analysis of melamine in food products. (pdf) 

Official Methods
FDA LIB4421: Determination of Melamine and Cyanuric Acid in Infant Formula using LC-MS/MS
FDA LIB4422: Interim Method for Melamine and Cyanuric Acids in Food using LC-MS/MS
FDA LIB4423: Melamine and Related Compounds GC-MS Screen
Europa JRC Detect Melamine in Food

Literature & References
FDA GC-MS Screen for Detection of Melamine, Ammeline, Ammelide, and Cyanuric Acid v2.1
FDA GC-MS Method for Screening and Confirmation of Melamine and Related Analogs

Related Products
SPE Tubes
  Discovery DSC-SCX SPE Cartridge, 500 mg/6 mL (52688-U)
HPLC Columns
  Ascentis® Express HILIC HPLC Column, 5 cm x 2.1 mm I.D., 2.7 µm particles (53934-U)
  Ascentis Express HILIC HPLC Column, 10 cm x 2.1 mm I.D., 2.7 µm particles (53939-U )
GC-MS Columns
  SLB-5ms Capillary Column, 30 m x 0.25 mm I.D., 0.25 µm (28471-U)
Analytical Standards
  Cyanuric acid analytical standard, =98.0% (HPLC) (16614)
  Melamine analytical standard, =99.0% (HPLC) (52549)
  Melamine solution 100 µg/mL in acetonitrile: water (1:1) (44642-U)
  Melamine-13C3 VETRANAL®, analytical standard (32666)
  Melamine-triamine-15N3 80-90 atom % 15N (triamine), 10-20 atom % 15N (triazine) (592889)

 


Diethylene Glycol (DEG) back to top

The chemical adulterant diethylene glycol (DEG), used as a substitute for glycerol, has been found in pharmaceuticals and consumer products like toothpastes, in OTC syrup products, and also in sweet wines in order increase the sweetness of taste; however, it has deadly toxic effects. DEG adulteration continues to this day, with a recent incident in Nigeria reportedly casing the deaths of 84 children who ingested teething syrup that was contaminated with DEG.


Applications
Glycols by GC

Literature & References
FDA GC-MS Screening Procedure for Presence of DEG and EG in Toothpaste

Related Products
GC Columns
  Nukol™ Capillary Column, 15 m × 0.53 mm I.D., 0.5 µm (25326)
Analytical Standards, Diol & Glycols
  Diethylene glycol, puriss. p.a., standard for GC, =99.5% (GC) (03128)
  2,3-Butanediol, puriss., mixture of racemic and meso forms, =99.0% (GC) (18970)
  1,2-Propanediol, puriss. p.a., standard for GC, =99.7% (GC) (12279)
  Ethylene glycol, puriss. p.a., standard for GC, =99.9% (GC) (85978)
  Dipropylene glycol, 99%, mixture of isomers (D215554)
  1,4-Butanediol, ReagentPlus®, =99% (240559)
  Triethylene glycol, ReagentPlus®, 99% (T59455)
  Glycerol, 99% (GC) (G9012)
  Tetraethylene glycol, 99% (110175)

 


Malachite Green Dye (MG) back to top

Malachite Green (MG) is a triphenylmethane compound primarily used as a dye or bacterial stain. It also has other applications; for example, in aquaculture for treatment of parasites, fungal and bacterial infections in fish and fish eggs. Due to its toxicity and potential carcinogenic effects it has been banned (since 1983) in the US from use to treat ailments in fish that are part of our food chain. Once malachite green is absorbed into fish tissue from the water source, it enters the fatty region and reduces to leucomalachite green (LMG). Although it has been banned in many countries, its use is ongoing in Asian countries, including China, where regulations are less stringent. As a requirement of the European Commission decision 2002/657/EC, a test method must be able to detect 2 µg/kg (ppb) of MG + LMG per kilogram of fish muscle.


Applications
Colors of the World, Fast Separation of Dyes with Ascentis Express,  Reporter 27.3 (pdf)

Official Methods - Malachite Green and Metabolites; Crystal Violet and Brilliant Green
FDA LIB4333-Leucomalachite Green in Salmon
FDA LIB4334-Determination of Malachite Green in Salmon with In-Situ Oxidation and LC w/ Visible Detection
FDA LIB4363-Quantitative and Confirmatory Analysis of Malachite Green and Leucomalachite Green Residues in Fish and Shrimp
FDA LIB4333 and 4334 Amendments-Application of Laboratory Information Bulletins for the Determination of Leucomalachite Green and Malachite Green Residues in Catfish, Basa, Tilapia, Trout, and Shrimp
FDA LIB4395-Analyses of Crystal Violet and Brilliant Green

Literature & References
FDA Malachite Green and Metabolites
Canadian Food Inspection Agency - Malachite Green

Related Products
HPLC Columns
  Ascentis® Express C8 HPLC Column, 10 cm x 4.6 mm I.D., 2.7 µm particles (53837-U)
Analytical Standards
  Malachite Green Chloride, 25 mg (38800)
  Food Residue Dyes

 


Antimicrobial Agents - Chloramphenicol & Fluoroquinolones back to top

Chloramphenicol

Chloramphenicol is a potent, broad-spectrum antibiotic and a potential carcinogen used only in therapeutic doses for treatment of serious infections in humans. Due to the unpredictable effect of dosage on different patient populations, it has not been possible to identify a safe level of human exposure. Hence, federal regulations in the United States, Canada and the European Union prohibit its use in food producing animals and animal-feed products, including honeybees. The FDA has increased the sampling of imported shellfish, honey, royal jelly, animal feed and milk products for detection of Chloramphenicol.


Applications
Chloramphenicol in Milk Using SupelMIP SPE
Antibacterials/Antifungals on Ascentis C18
Applications by Compound Class-Drugs

Official Methods
FDA methods for Residues of Chloramphenicol in Residues and Related Compounds in Food-Honey, Shrimp, Crab and Crawfish

Literature & References
UK Food Standards Agency - Chloramphenicol
Development of an improved method for trace analysis of chloramphenicol using molecularly imprinted polymers, Boyd, B, Björk H, Billing J, Shimelis O, Axelsson S, Leonora M, Yilmaz E, Journal of Chromatography A (2007), 1174(1-2):63-71
Advantages of molecularly imprinted polymers LC-ESI-MS/MS for the selective extraction and quantification of Chloramphenicol in milk-based matrices. Comparison between a classical sample preparation., Mohamed R, Richoz-Payot J, Gremaud E, Mottier P, Yilmaz E, Tabet JC and Guy P, Anal.Chem. (2007), 79(24), 9557-9565
The Selective Extraction of Chloramphenicol using Molecularly Imprinted Polymer SPE, Shimelis O, Trinh A, Brandes H, US Supelco Reporter, 25.1 (482 Kb PDF)
SupelMIP Literature and References

Related Products
SPE Tubes
  SupelMIP SPE - Chloramphenicol, 25 mg/10mL (LRC) (53210-U)
HPLC Columns
  Ascentis® C18, 15 cm x 4.6 mm I.D., 5 µm particles (581324-U )
  Ascentis C18, 10 cm x 2.1 mm I.D., 3 µm particles (581301-U)
Analytical Standards
  Chloramphenicol VETRANAL®, analytical standard (46110)
  Chloramphenicol palmitate VETRANAL®, analytical standard (46109)

Fluoroquinolones

Fluoroquinolones are among the earliest man-made or synthesized antibiotics commonly used to treat bacterial infections and acute respiratory diseases. They are used in both humans and animals and have a wide range of effects. Most commonly prescribed fluoroquinolones in use are Ciprofloxacin (broad-spectrum antibiotic used extensively since 1980 with few restrictions), Enrofloxacin (anti-inflammatory drug used in animals), Sarafloxacin, Difloxacin, Danofloxacin, Enoxacin, Fleroxacin, Norfloxacin, Ofloxacin, Sparfloxacin, Flumequin, Marbofloxacin, and Oxolinic acid. Residues of fluoroquinolones, particularly of Ciprofloxacin and Enrofloxacin have been found in excessive quantities in frozen seafood from China, Vietnam and other Asian countries. Application of fluoroquinolones in apiculture as a prophylaxis for bee diseases is highly conceivable and residues in honey samples have been found. The human body does exhibit adverse reactions to fluoroquinolones; also, adsorption into human tissues can lead to resistance against antibiotics and cause health complications.


Applications
The Selective Extraction of Fluoroquinolones in Veterinary Samples Using Molecularly Imprinted Polymer SPE (462kb pdf)
Fluoroquinolone antibiotics application for HPLC G003713

Official Methods
FDA Laboratory Methods: Fluoroquinolones in Food
USDA Food Safety Inspection Service (FSIS) Confirmation of Fluoroquinolones Antibiotics by Ion Mass Spectroscopy (pdf)

Literature & References
Fluoroquinolones SupelMIP Product Information Sheet (pdf)

Related Products
SPE Tubes
  SupelMIP SPE – Fluoroquinolones 25 mg/3 mL (53269-U)
HPLC Columns
  Ascentis C18, 5 cm x 3 mm I.D., 3 µm particle size, w/Guard Column (581307-U)
Analytical Standards
  Quinolones & Fluoroquinolones