TY - JOUR
T1 - Determination of methylglyoxal-bis(guanylhydrazone) in body fluids by ion-pair chromatography
AU - Roboz, J.
AU - Wu, K. T.
AU - Hart, R. D.
N1 - Funding Information:
This work was partially supported by Contracts CM-53837 and CM-97294, and Grant CA-15936 from the National Cancer Institute, National Institute of Health, USA.
PY - 1980
Y1 - 1980
N2 - Methylglyoxal-bis(guanylhydrazone), Methyl-G, is a potent antineoplastic agent currently undergoing phase I clinical trials. Serum, ascitic and pleural fluids, and urine are deproteinized with methanol, supernatant is evaporated, residue is redissolved in the eluent, lipids are removed with carbon tetrachloride, and an aliquot of the aqueous layer injected into the chromatograph. Ethylglyoxal-bis(guanylhydrazone) (Ethyl-G) is the internal standard. The mobile phase is a mixture of an aqueous buffer (containing 0.004 M heptane and pentane sulfonic acid, 90%:10%, buffered to pH 3.5) and methanol (68%:32%). The ion-pair complex is retained on a μBondapak C18 column, eluted with a flow of 2.0 ml/min. Absorbance is measured at 280 nm. Detectability: 30 ng/ml (0.11 μM) in serum, ascitic and pleural fluids, 300 ng/ml (1.1 μM) in urine. Calibration curves (peak height ratios of Methyl-G/Ethyl-G plotted against known drug concentrations) were linear in the 0.1-30 μg/ml range. Correlation coefficients were 0.999; coefficients of variation for reproducibility were <5%. Residual blood levels of Methyl-G persist for several days. Methyl-G was found to pass into ascitic fluid.
AB - Methylglyoxal-bis(guanylhydrazone), Methyl-G, is a potent antineoplastic agent currently undergoing phase I clinical trials. Serum, ascitic and pleural fluids, and urine are deproteinized with methanol, supernatant is evaporated, residue is redissolved in the eluent, lipids are removed with carbon tetrachloride, and an aliquot of the aqueous layer injected into the chromatograph. Ethylglyoxal-bis(guanylhydrazone) (Ethyl-G) is the internal standard. The mobile phase is a mixture of an aqueous buffer (containing 0.004 M heptane and pentane sulfonic acid, 90%:10%, buffered to pH 3.5) and methanol (68%:32%). The ion-pair complex is retained on a μBondapak C18 column, eluted with a flow of 2.0 ml/min. Absorbance is measured at 280 nm. Detectability: 30 ng/ml (0.11 μM) in serum, ascitic and pleural fluids, 300 ng/ml (1.1 μM) in urine. Calibration curves (peak height ratios of Methyl-G/Ethyl-G plotted against known drug concentrations) were linear in the 0.1-30 μg/ml range. Correlation coefficients were 0.999; coefficients of variation for reproducibility were <5%. Residual blood levels of Methyl-G persist for several days. Methyl-G was found to pass into ascitic fluid.
UR - http://www.scopus.com/inward/record.url?scp=0018863126&partnerID=8YFLogxK
U2 - 10.1093/jat/4.3.127
DO - 10.1093/jat/4.3.127
M3 - Article
C2 - 6999237
AN - SCOPUS:0018863126
SN - 0146-4760
VL - 4
SP - 127
EP - 131
JO - Journal of Analytical Toxicology
JF - Journal of Analytical Toxicology
IS - 3
ER -