Determination of 18 phthalate metabolites in human urine using a liquid chromatography-tandem mass spectrometer equipped with a core–shell column for rapid separation

2015 ◽  
Vol 7 (19) ◽  
pp. 8048-8059 ◽  
Author(s):  
Yong-Lai Feng ◽  
Xiangjun Liao ◽  
Genevieve Grenier ◽  
Nathalie Nguyen ◽  
Peter Chan
Keyword(s):  
Liquid Chromatography ◽  
Mass Spectrometer ◽  
Human Urine ◽  
Core Shell ◽  
Tandem Mass ◽  
Rapid Separation ◽  
Tandem Mass Spectrometer ◽  
Phthalate Metabolites ◽  
Liquid Chromatography Tandem Mass

Phthalates are a group of chemicals used in a variety of products worldwide.

scholarly journals RAPID, METHOD FOR DETERMINATION OF METFORMIN AND CANAGLIFLOZIN IN PLASMA BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETER, APPLICATION TO BIOEQUIVALENCE STUDY

2019 ◽  
pp. 93-97
Author(s):  
SAMBASIVA RAO PURAM ◽  
NITHYA G ◽  
SUBBA RAO NB ◽  
RAMAN BATHEJA
Keyword(s):  
Liquid Chromatography ◽  
Mass Spectrometer ◽  
Mobile Phase ◽  
Solid Phase ◽  
Bioequivalence Study ◽  
Simultaneous Estimation ◽  
Tandem Mass ◽  
Tandem Mass Spectrometer ◽  
Liquid Chromatography Tandem Mass

Objective: The objective of the study was to develop and validate a rapid selective bioanalytical method for the simultaneous determination of metformin and canagliflozin in plasma by liquid chromatography-tandem mass spectrometer (LC-MS/MS) to facilitate bioequivalence study sample analysis. Stock solutions and spiking solutions were prepared accurately in methanol and 80% methanol in water, respectively. Methods: Chromatography monitored using Analyst 1.6.2 software. Method was found selective, no matrix effect, reproducible and consistent recovery, accuracy, precision, and stable in aqueous as well as extracted/matrix samples. Method found linear over the range 10–2000 ng/ml for metformin and 30–6000 ng/ml for canagliflozin. The method is successfully applied to analyze samples collected in a bioequivalence study after administration of metformin/canagliflozin 1000/150 mg to 24 healthy male volunteers. Results: Extraction was carried out using a simple solid phase extraction using mobile phase elution. 5 μl sample delivered as injection volume in 1.000 ml/min isocratic mobile phase flow on turbo ion electron spray technique for positive mode on API 4000 MS. Discussion: Chromatography achieved within 3 min using a mobile phase containing acetonitrile and 10 mM ammonium formate buffer in a ratio of 70:30 on chromolith C18 analytical column. Q1/Q3 are 130.1/70.1, 136.3/77.1, 462.2/267.2 (with ammonium adduct), and 466.4/267.1 for metformin, metformin D6, canagliflozin, and canagliflozin D4, respectively. Conclusion: Rapid, sensitive method for the simultaneous estimation of metformin and canagliflozin in plasma by LC-MS/MS is successfully developed, validated and applied to analyze 960 unknown samples of a bioequivalence study. Incurred sample reanalysis was revealed great reproducibility.

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