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Validation of a rapid method of analysis using ultrahigh-performance liquid chromatography - tandem mass spectrometry for nitrogen-rich adulterants in nutritional food ingredients.

Journal of chromatography. A (2014-12-02)
Jon Draher, Vickie Pound, Todime M Reddy
ABSTRACT

A method for the rapid quantification of 9 potential nitrogen-rich economic adulterants (dicyandiamide, urea, biuret, cyromazine, amidinourea, ammeline, amidinourea, melamine, and cyanuric acid) in five milk and soy derived nutritional ingredients, i.e. whole milk powder, nonfat dry milk, milk protein concentrate, sodium caseinate, and soy protein isolate has been developed and validated for routine use. The samples were diluted tenfold with water followed by treatment with 2% formic acid and acetonitrile to precipitate proteins. Sample extracts were analyzed using hydrophilic interaction chromatography and tandem mass spectrometry (HILIC-MS/MS) under both positive and negative modes. Stable isotope labeled internal standards were used to ensure accurate quantification. In multi-day validation experiments, the average accuracies, relative standard deviations (RSD), and method detection limits (MDL) for all analytes in whole milk powder were 82-101%, 6-13%, and 0.1mg/kg-7 mg/kg, respectively. The retention times of the analytes in matrix spiked controls were within ± 0.06 min of the average retention times of the corresponding analytes in calibration standards. The validated method was proven to be rugged for routine use to quantify the presence of 9 nitrogen-rich compounds in milk and soy derived ingredients and to provide a defense from economically motivated adulteration.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
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Formic acid, reagent grade, ≥95%
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Acetonitrile, HPLC Plus, ≥99.9%
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Urea, powder, BioReagent, for molecular biology, suitable for cell culture
Supelco
Ammonium acetate, suitable for mass spectrometry (MS), LiChropur, eluent additive for LC-MS
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Ammonium acetate, for molecular biology, ≥98%
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Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
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Urea, ACS reagent, 99.0-100.5%
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Melamine, 99%
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Formic acid, ACS reagent, ≥96%
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Acetonitrile, for HPLC, for UV, ≥99.9% (GC)
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Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
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Urea, ReagentPlus®, ≥99.5%, pellets
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Dicyandiamide, 99%
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Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
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Ammonium acetate, ACS reagent, ≥97%
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Acetonitrile, ACS reagent, ≥99.5%
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Ammonium acetate, reagent grade, ≥98%
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Ammonium acetate solution, for molecular biology, 7.5 M
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Ammonium acetate, ≥99.99% trace metals basis
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Urea solution, BioUltra, ~8 M in H2O
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Metformin Related Compound A, Pharmaceutical Secondary Standard; Certified Reference Material
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Urea, BioXtra, pH 7.5-9.5 (20 °C, 5 M in H2O)
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Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Supelco
Melamine, analytical standard
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Urea, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99%

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