TY - JOUR
T1 - Determination of pamidronate in urine by ion-pair liquid chromatography after derivatization with 1-naphthylisothiocyanate
AU - Sparidans, Rolf W.
AU - Den Hartigh, Jan
AU - Beijnen, Jos H.
AU - Vermeij, Pieter
PY - 1997/8/15
Y1 - 1997/8/15
N2 - A sensitive method for the determination of pamidronate disodium [(3-amino-1-hydroxypropylidene)bisphosphonate, APD] in urine has been developed and validated. The procedure involves a triple co-precipitation with calcium phosphate, solid-phase extraction on a quaternary ammonium column, derivatization with 1-naphthylisothiocyanate and ion-pair liquid-liquid extraction. From the two reaction products, naphthylthiocarbamyl-APD is converted into the other, naphthylcarbamyl-APD, by an oxidative desulphuration with hydrogen peroxide prior to analysis by ion-pair HPLC and fluorescence detection at 285/390 nm. The method has a coefficient of variation of 7% for the intra-assay precision of 99 ng ml-1 APD and 11% for the inter-assay precision. The lower limit of quantification is 3 ng ml-1 APD in 2.5 ml of human urine.
AB - A sensitive method for the determination of pamidronate disodium [(3-amino-1-hydroxypropylidene)bisphosphonate, APD] in urine has been developed and validated. The procedure involves a triple co-precipitation with calcium phosphate, solid-phase extraction on a quaternary ammonium column, derivatization with 1-naphthylisothiocyanate and ion-pair liquid-liquid extraction. From the two reaction products, naphthylthiocarbamyl-APD is converted into the other, naphthylcarbamyl-APD, by an oxidative desulphuration with hydrogen peroxide prior to analysis by ion-pair HPLC and fluorescence detection at 285/390 nm. The method has a coefficient of variation of 7% for the intra-assay precision of 99 ng ml-1 APD and 11% for the inter-assay precision. The lower limit of quantification is 3 ng ml-1 APD in 2.5 ml of human urine.
KW - 1-Naphthylisothiocyanate
KW - Bisphosphonates
KW - Pamidronate
UR - http://www.scopus.com/inward/record.url?scp=0030767907&partnerID=8YFLogxK
U2 - 10.1016/S0378-4347(97)00226-0
DO - 10.1016/S0378-4347(97)00226-0
M3 - Article
C2 - 9300918
AN - SCOPUS:0030767907
SN - 1572-6495
VL - 696
SP - 137
EP - 144
JO - Journal of chromatography. B, Biomedical applications
JF - Journal of chromatography. B, Biomedical applications
IS - 1
ER -