Highly sensitive assay for the determination of therapeutic peptide desmopressin in human plasma by UPLC–MS/MS  

作　　者：Shiva Kumar Gudlawar Nageswara Rao Pilli Sridhar Siddiraju Jaya Dwivedi 

机构地区：[1]Department of Chemistry,Banasthali Vidyapeeth,Jaipur 304022,India [2]Wellquest Clinical Research Laboratories,Ramanthapur,Hyderabad 500013,India [3]Department of Pharmaceutical Chemistry,Malla Reddy College of Pharmacy,Maisammaguda,Secunderabad 5000100,India

出　　处：《Journal of Pharmaceutical Analysis》2017年第3期196-202,共7页药物分析学报（英文版）

摘　　要：An analytical method based on ultra-performance liquid chromatography with positive ion electrospray ionization(ESI) coupled with tandem mass spectrometry(UPLC–MS/MS) was developed and validated for the determination of therapeutic peptide desmopressin in human plasma. A desmopressin stable labeled isotope(desmopressin d_8) was used as an internal standard. Analyte and the internal standard were extracted from200 μL of human plasma via solid-phase extraction technique using Oasis WCX cartridges. The chromatographic separation was achieved on an Aquity UPLC HSS T3 column by using a gradient mixture of methanol and 1 m M ammonium formate buffer as the mobile phase. The calibration curve obtained was linear(r^2≥0.99)over the concentration range of 1.01–200 pg/m L. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The results of the intra-and inter-day precision and accuracy studies were well within the acceptable limits. The proposed method was successfully applied to pharmacokinetic studies in humans.An analytical method based on ultra-performance liquid chromatography with positive ion electrospray ionization(ESI) coupled with tandem mass spectrometry(UPLC–MS/MS) was developed and validated for the determination of therapeutic peptide desmopressin in human plasma. A desmopressin stable labeled isotope(desmopressin d_8) was used as an internal standard. Analyte and the internal standard were extracted from200 μL of human plasma via solid-phase extraction technique using Oasis WCX cartridges. The chromatographic separation was achieved on an Aquity UPLC HSS T3 column by using a gradient mixture of methanol and 1 m M ammonium formate buffer as the mobile phase. The calibration curve obtained was linear(r^2≥0.99)over the concentration range of 1.01–200 pg/m L. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The results of the intra-and inter-day precision and accuracy studies were well within the acceptable limits. The proposed method was successfully applied to pharmacokinetic studies in humans.

关 键 词：DESMOPRESSIN SOLID-PHASE extraction (SPE) Ultra performance liquid chromatography–tandem mass SPECTROMETRY Method validation PHARMACOKINETICS 

分 类 号：R969[医药卫生—药理学]