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Simultaneous determination of ethylene glycol and glycolic acid in serum by gas chromatography-mass spectrometry.
J Anal Toxicol. 1999 Nov-Dec; 23(7):591-7.JA

Abstract

We describe a gas chromatographic-mass spectrometric (GC-MS) procedure for the simultaneous determination of ethylene glycol (EG) and its major toxic metabolite, glycolic acid (GA), in serum. In this method, serum (50 microL) is treated with 150 microL of glacial acetic acid/acetonitrile (1:10, v/v; contains internal standard, 1,3-propanediol, 15 mg/dL) to precipitate protein. After centrifugation, 10 microL of supernate is treated with 500 microL of 2,2-dimethoxypropane/dimethylformamide (80:20, v/v) to convert water to methanol, and the volume is then reduced to < 100 microL of dimethylformamide (but not to dryness). After formation of tertbutyldimethylsilyl derivatives, analysis is performed by capillary column GC-MS in selected ion mode. The method gives a linear response to 1000 mg/L each EG and GA (16.1 mmol/L and 13.2 mmol/L, respectively) and has a lower limit of detection and a lower limit of quantitation of 10 mg/L each EG and GA (0.16 mmol/L and 0.13 mmol/L, respectively). Total assay imprecision is CV < or = 6.4% (200 and 800 mg/L EG and GA [3.2 and 12.9 mmol/L EG; 2.6 and 10.5 mmol/L GA, respectively]). Absolute recovery from human serum was 91.1% for EG and 77.6% for GA. The procedure is free from any known interference. A complete analysis set (three calibrators, patient serum neat, patient serum diluted 1:5 (v/v), and two controls) may be completed in about 2 h. A preliminary result, based on a single calibrator and patient serum diluted 1:5 (v/v), is complete in about 1 h. The method has been used to aid the diagnosis and management in 34 cases of EG intoxication. Selected cases are briefly reviewed.

Authors+Show Affiliations

Department of Pathology and Laboratory Medicine, University of Kentucky Medical Center, Lexington 40536-0293, USA. wporter@pop.uky.eduNo affiliation info availableNo affiliation info available

Pub Type(s)

Case Reports
Journal Article

Language

eng

PubMed ID

10595845

Citation

Porter, W H., et al. "Simultaneous Determination of Ethylene Glycol and Glycolic Acid in Serum By Gas Chromatography-mass Spectrometry." Journal of Analytical Toxicology, vol. 23, no. 7, 1999, pp. 591-7.
Porter WH, Rutter PW, Yao HH. Simultaneous determination of ethylene glycol and glycolic acid in serum by gas chromatography-mass spectrometry. J Anal Toxicol. 1999;23(7):591-7.
Porter, W. H., Rutter, P. W., & Yao, H. H. (1999). Simultaneous determination of ethylene glycol and glycolic acid in serum by gas chromatography-mass spectrometry. Journal of Analytical Toxicology, 23(7), 591-7.
Porter WH, Rutter PW, Yao HH. Simultaneous Determination of Ethylene Glycol and Glycolic Acid in Serum By Gas Chromatography-mass Spectrometry. J Anal Toxicol. 1999 Nov-Dec;23(7):591-7. PubMed PMID: 10595845.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of ethylene glycol and glycolic acid in serum by gas chromatography-mass spectrometry. AU - Porter,W H, AU - Rutter,P W, AU - Yao,H H, PY - 1999/12/14/pubmed PY - 1999/12/14/medline PY - 1999/12/14/entrez SP - 591 EP - 7 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 23 IS - 7 N2 - We describe a gas chromatographic-mass spectrometric (GC-MS) procedure for the simultaneous determination of ethylene glycol (EG) and its major toxic metabolite, glycolic acid (GA), in serum. In this method, serum (50 microL) is treated with 150 microL of glacial acetic acid/acetonitrile (1:10, v/v; contains internal standard, 1,3-propanediol, 15 mg/dL) to precipitate protein. After centrifugation, 10 microL of supernate is treated with 500 microL of 2,2-dimethoxypropane/dimethylformamide (80:20, v/v) to convert water to methanol, and the volume is then reduced to < 100 microL of dimethylformamide (but not to dryness). After formation of tertbutyldimethylsilyl derivatives, analysis is performed by capillary column GC-MS in selected ion mode. The method gives a linear response to 1000 mg/L each EG and GA (16.1 mmol/L and 13.2 mmol/L, respectively) and has a lower limit of detection and a lower limit of quantitation of 10 mg/L each EG and GA (0.16 mmol/L and 0.13 mmol/L, respectively). Total assay imprecision is CV < or = 6.4% (200 and 800 mg/L EG and GA [3.2 and 12.9 mmol/L EG; 2.6 and 10.5 mmol/L GA, respectively]). Absolute recovery from human serum was 91.1% for EG and 77.6% for GA. The procedure is free from any known interference. A complete analysis set (three calibrators, patient serum neat, patient serum diluted 1:5 (v/v), and two controls) may be completed in about 2 h. A preliminary result, based on a single calibrator and patient serum diluted 1:5 (v/v), is complete in about 1 h. The method has been used to aid the diagnosis and management in 34 cases of EG intoxication. Selected cases are briefly reviewed. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/10595845/Simultaneous_determination_of_ethylene_glycol_and_glycolic_acid_in_serum_by_gas_chromatography_mass_spectrometry_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/23.7.591 DB - PRIME DP - Unbound Medicine ER -