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A new simple, specific, and selective bioanalytical method was established for the concurrent quantification of Empagliflozin, Dapagliflozin, Metformin, and Linagliptin in spiked human blood plasma by RPLC-MS/MS and validated as per the USFDA guidelines. The enrichment of analytes from the plasma was accomplished by protein precipitation method by using Methyl alcohol. By adopting our method one can achieve the separation and estimation of Empagliflozin, Dapagliflozin, Metformin, and Linagliptin in combination forms, where one drug can act as an internal standard. The analytes were separated and analyzed by triple quadrupole mass spectrometer using photomultiplier tube as a detector, with the electron spray ionization technique of positive and negative mode on Zorbax SB octadecyl silica column (50mm x 3.6 mm i.d., 5µm) with a moving phase (10mMAmmonium Acetate Buffer (pH-5): Cyanomethane 20:80 v/v) at a 0.5 ml/min flow rate, with a run time of 5.0 min A Linear calibration plotted in the concentration range 7.5-150ng/ml (Empagliflozin), 15.8-316ng/ml (Dapagliflozin), 6-120ng/ml(Metformin). LOD was found to be 2.450, 5.200, 1.95ng/ml, and LOQ were found to be 7.5, 1.50, 6.0 ng/ml for Empagliflozin, Dapagliflozin, and Metformin respectively. The Regression Coefficient was found to be 0.992, 0.996, and 0.995 for respective drugs. The established method was accurate and precise as per USFDA guidance for the industry, useful for Pharmacokinetic study and Bioequivalence study. [ABSTRACT FROM AUTHOR]

A simple, rapid, specific and sensitive method has been proposed for the development and validation of bio- analytical method for the concurrent quantification of hydrochlorothiazide and valsartan using losartan as an internal standard in human blood plasma by LC-MS/MS. The separation was achieved using ZORBAX SB CI8 (5pmx50x3.6mm i.d.), mobile phase containing Cyanomethane: Ammonium Formate (70:30v/v) pH adjusted to 4.25 and flow rate of the mobile phase was 0.5ml/min and the injection volume I0pl and the column oven temperature is ambient. The retention time of hydrochlorothiazide (HCT) and valsartan (VST) was found to be 1.22 and 1.08min, respectively. The developed method was found to be linear over the concentration range of 420-8400 (r2 value 0.9932) and 6-I22ng/ml (r2 value 0-9954) using losartan as internal standard. LOD and LOQ of valsartan I and 3ng/ml and that of hydrochlorothiazide was 0.5 and 2 ng/ml respectively. Shimadzu LC-MS/MS 8030 was configured with Lab solution data solution, Triple quadrupole analyzer, ESI interface. Hydrochlorothiazide and valsartan were extracted by Liquid-Liquid extraction method. According to USFDA guidelines the method was established and validated. This method can applicable for the Pharmacokinetic, Bioequivalence and Bioavailability studies contains valsartan and hydrochlorothiazide. [ABSTRACT FROM AUTHOR]

A simple, selective method was developed for simultaneous estimation of Cefixime, Ornidazole and Dicloxacillin in blood plasma and validated as per the US FDA guidelines. Extraction process was accomplished by protein precipitation method. By employing cefixime as internal standard in methyl alcohol solvent, the proteins got precipitated. Single method can be used for separating combination drugs, where any one drug can act as an internal standard. The drugs were analyzed by triple quadrupole mass spectrometer using photomultiplier tube as detector, with the electron spray ionization technique of positive and negative mode on a shim-pack solar C18(50 x 4.6mm i.d, 5µm) column. The mobile phase comprising of 10mM ammonium acetate and Methyl alcohol with the ratio 10:90v/v, pH 6.0. After the evaluation of different sample pretreatment techniques, protein precipitation was found to be satisfactory, offering good recovery values. The linearity of Ornidazole and Dicloxacillin found within range of 4.0 - 80.0µg/ml and 1.5 - 30.0µg/ml respectively which is consistently accurate for plotting curve. The correlation coefficient of Ornidazole and Dicloxacillin were 0.9936 and 0.9994 respectively. The Limit of detection of Ornidazole and Dicloxacillin was found to be 330ng/ml and 123.5ng/ml respectively and their Limit of quantification values were 1000ng/ml and 375ng/ml respectively. Different constituents of plasma will not affect the effective recovery of the drugs. The established method can be used for the quantification of drugs in plasma for BA-BE studies and biopharmaceutical sciences. [ABSTRACT FROM AUTHOR]