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Determination of N-nitrosodiethanolamine, NDELA in cosmetic ingredients and products by mixed mode solid phase extraction and UPLC-tandem mass spectrometry with porous graphitic carbon column through systemic sample pre-cleanup procedure

Title
Determination of N-nitrosodiethanolamine, NDELA in cosmetic ingredients and products by mixed mode solid phase extraction and UPLC-tandem mass spectrometry with porous graphitic carbon column through systemic sample pre-cleanup procedure
Authors
Joo, Kyung-MiShin, Mi-SookJung, Ji-HeeKim, Boo-MinLee, John-WhanJeong, Hye-JinLim, Kyung-Min
Ewha Authors
임경민
SCOPUS Author ID
임경민scopus
Issue Date
2015
Journal Title
TALANTA
ISSN
0039-9140JCR Link1873-3573JCR Link
Citation
vol. 137, pp. 109 - 119
Keywords
N-nitrosodiethanolamine (NDELA)Mixed mode solid phase extractionPorous graphitic carbon (PGC) columnUPLC-MS/MSCosmetics
Publisher
ELSEVIER SCIENCE BV
Indexed
SCI; SCIE; SCOPUS WOS
Abstract
A rapid, sensitive, accurate and specific ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method for the detection of N-nitrosodiethanolamine (NDELA), a highly toxic contaminant in cosmetic raw materials and products was developed and validated. Systematized sample preparation steps were developed according to product types. Various SPE cartridges and columns were examined to establish the condition of SPE and chromatographic separation for NDELA. Sample cleanup steps consisting of solvent and liquid-liquid extraction tailored to the various sample matrix types were established prior to mixed mode SPE (Bond Elut AccuCAT). Chromatographic separation was achieved within 7 min on a porous graphitic carbon (PGC) column using a gradient elution with the mobile phase of 1 mM ammonium acetate containing 0.1% acetic acid and methanol. NDELA was monitored using an electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode (m/z 134.9 > 103.7(quantifier) and 73.7(qualifier ion)) with d8-NDELA (m/z 143.1 > 111.0) as internal standard. The standard curves were linear over the concentration range of 1-100 ng/mL with a correlation coefficient higher than 0.99. The limit of detection CLOD) and the limit of quantification (LOQ) was 10 and 20 mu g/kg, respectively (0.5 and 1 ng/mL in standard solution). The intra- and inter-day precisions were estimated to be below 11.1% and accuracies were within the range of 90.8-115.8%. The validated method was successfully applied to the analysis of real samples including raw materials, skin care, make-up, shampoos and hair products. (C) 2015 Elsevier B.V. All rights reserved.
DOI
10.1016/j.talanta.2015.01.019
Appears in Collections:
약학대학 > 약학과 > Journal papers
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