A novel and sensitive method for ethinylestradiol quantification in human plasma by high-performance liquid chromatography coupled to atmospheric pressure photoionization (APPI) tandem mass spectrometry: Application to a comparative pharmacokinetics study

Borges, Ney Carter do Carmo; Astigarraga, Rafael Barrientos; Sverdloff, Carlos Eduardo; Galvinas, Paulo Rabelo; Silva, Washington Moreira da; Rezende, Vinícius Marcondes; Moreno, Ronílson Agnaldo

doi:10.1016/j.jchromb.2009.08.048

Cited by 19 publications

(20 citation statements)

References 35 publications

(45 reference statements)

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“…To avoid interlaboratory bias in establishing an appropriate bioanalytical error model, the data set was combined with a similar‐sized data set obtained from bioanalysis validation reports published in 2009 in J Chromatogr B Analyt Technol Biomed Life Sci that contained information on the interday precision at the LLOQ and a low–mid–high concentration range (Borges et al. ; Carli et al. ; Clavijo et al.…”

Section: Methodsmentioning

confidence: 99%

“…To obtain a credible model for the part of the residual error describing the bioanalytical uncertainty, we reviewed published data on interday precision from validation studies performed in our own laboratory (Vainchtein et al 2006a(Vainchtein et al ,b, 2007ater Heine et al 2007ter Heine et al , 2009Damen et al 2008Damen et al , 2009aJansen et al 2009Jansen et al , 2010. To avoid interlaboratory bias in establishing an appropriate bioanalytical error model, the data set was combined with a similar-sized data set obtained from bioanalysis validation reports published in 2009 in J Chromatogr B Analyt Technol Biomed Life Sci that contained information on the interday precision at the LLOQ and a low-mid-high concentration range (Borges et al 2009;Carli et al 2009;Clavijo et al 2009;Gu et al 2009;Ling et al 2009;Nirogi et al 2009a,b;Qiao et al 2009;Zhang et al 2009;Ptolemy et al 2010;Stanton et al 2010). To these validation data, a mean error model of the form y = ax + b was fitted, in which x is the ratio of the nominal concentration relative to the LLOQ, y is the absolute error, calculated as the reported relative interday uncertainty at nominal concentration x multiplied by x, a defines the part of the error proportional to the concentration, and b is the additive part of the error.…”

Section: Simulation Studiesmentioning

confidence: 99%

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Incorporation of concentration data below the limit of quantification in population pharmacokinetic analyses

Keizer

Jansen

Rosing

et al. 2015

Pharmacology Res & Perspec

145

137

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Handling of data below the lower limit of quantification (LLOQ), below the limit of quantification (BLOQ) in population pharmacokinetic (PopPK) analyses is important for reducing bias and imprecision in parameter estimation. We aimed to evaluate whether using the concentration data below the LLOQ has superior performance over several established methods. The performance of this approach (“All data”) was evaluated and compared to other methods: “Discard,” “LLOQ/2,” and “LIKE” (likelihood-based). An analytical and residual error model was constructed on the basis of in-house analytical method validations and analyses from literature, with additional included variability to account for model misspecification. Simulation analyses were performed for various levels of BLOQ, several structural PopPK models, and additional influences. Performance was evaluated by relative root mean squared error (RMSE), and run success for the various BLOQ approaches. Performance was also evaluated for a real PopPK data set. For all PopPK models and levels of censoring, RMSE values were lowest using “All data.” Performance of the “LIKE” method was better than the “LLOQ/2” or “Discard” method. Differences between all methods were small at the lowest level of BLOQ censoring. “LIKE” method resulted in low successful minimization (<50%) and covariance step success (<30%), although estimates were obtained in most runs (∼90%). For the real PK data set (7.4% BLOQ), similar parameter estimates were obtained using all methods. Incorporation of BLOQ concentrations showed superior performance in terms of bias and precision over established BLOQ methods, and shown to be feasible in a real PopPK analysis.

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Section: Methodsmentioning

confidence: 99%

Section: Simulation Studiesmentioning

confidence: 99%

Incorporation of concentration data below the limit of quantification in population pharmacokinetic analyses

Keizer

Jansen

Rosing

et al. 2015

Pharmacology Res & Perspec

145

137

View full text Add to dashboard Cite

show abstract

“…II). This technique has been used in the past to ionize less polar biochemicals, such as sterols and steroids (28)(29)(30)(31)(32)(33)(34). The ionization mechanism is somewhat different from electrospray because in most cases a dopant is used to provide the proton to complete the ionization process.…”

Section: Gc/ms Of Total Plasma Palmitate and Cholesterolmentioning

confidence: 99%

In vivo D2O labeling to quantify static and dynamic changes in cholesterol and cholesterol esters by high resolution LC/MS

Castro-Perez

Previs

McLaren

et al. 2011

Journal of Lipid Research

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high level of cholesterol in the body circulation is strongly associated with atherosclerosis ( 6-10 ). The source of cholesterol comes from different areas: dietary, de novo synthesis, and synthesis in extrahepatic tissues. The liver acts as a cross-junction at which cholesterol is incorporated into HDL/LDL, and then secreted as free cholesterol in the bile or in the form of bile salts/acids.Studies of cholesterol metabolism typically require measurements of static concentrations of cholesterol to identify differences between models or to determine the presence or absence of a disease phenotype. The simultaneous use of stable or radio isotope fl ux analysis can aid in understanding the nature of a metabolic abnormality and yield information regarding the dynamics that contribute to altered or perturbed homeostasis.Questions surrounding cholesterol dynamics have been addressed using isotopic-labeled water for nearly 70 years, beginning with the pioneering studies of Schoenheimer The liver plays a vital role in cholesterol metabolism ( 1-5 ) and homeostasis. In addition to this, production of bile acids from cholesterol also plays an important role in the secretion and degradation of plasma lipoproteins. A 25 September 2010. Published, JLR Papers in Press, September 30, 2010 DOI 10.1194 In vivo D2O labeling to quantify static and dynamic changes in cholesterol and cholesterol esters by high resolution LC/MS Manuscript received 27 July 2010 and in revised form

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“…The LC-MS/ MS method described here is specific due to the inherent selectivity of tandem mass spectrometry is in accordance with both Food and Drug Administration (FDA) and the National Sanitary Surveillance Agency (ANVISA) requirements for pharmacokinetic studies. This method offers the advantage over those previously reported using LC-MS/MS [24,27,29,48] showing a low validated LOQ 1 pg mL −1 (ethinylestradiol) and LOQ 50.64 pg mL −1 (gestodene).…”

Section: Discussionmentioning

confidence: 80%

“…Blood samples (06 mL) were collected by indwelling catheter into EDTA containing tubes before dosing and 15, 30, 45 min and also 1, 1.25, 1.5, 1.75, 2, 2.50, 3,4,6,8,12,16,24,36,48,72, 96 h post-dosing for ethinylestradiol and gestodene. The blood samples were centrifuged at 3.000 rpm for 10 min.…”

Section: Study Proceduresmentioning

confidence: 99%

Bioequivalence of Two Oral Contraceptive Drugs Containing Ethinylestradiol and Gestodene in Healthy Female Volunteers

Abib¹,

Duarte²,

Vanunci³

et al. 2010

JBB

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The bioavailability and bioequivalence of two different film coated tablets containing ethinylestradiol and gestodene were investigated in 36 healthy female volunteers after oral single-dose administration. The study was performed according to a single-center, randomized, single-dose, 2-way cross-over design with a wash-out phase of 28 days. Blood samples for pharmacokinetic profiling were taken postdose up to 72 h (ethinylestradiol) and 96 h (gestodene). Ethinylestradiol and gestodene plasma concentrations were determined with a validated LC-MS/MS method. Bioequivalence between the products was determined by calculating 90% confidence intervals (90% I.C) for the ratio of AUC 0-t and C max values for the test and reference products, using logarithmic transformed data. The 90% confidence intervals of ethinylestradiol were 98.49%-109.19%, and 100.62%-111.69%, respectively. The 90% confidence intervals of gestodene were 94.07%-105.91%, and 110.19%-124.73%, respectively. Since the 90% confidence intervals for C max and AUC 0-t were within the 80-125% interval proposed by Food and Drug Administration, it was concluded that the two ethinylestradiol and gestodene formulations are bioequivalent in their rate and extent of absorption.

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A novel and sensitive method for ethinylestradiol quantification in human plasma by high-performance liquid chromatography coupled to atmospheric pressure photoionization (APPI) tandem mass spectrometry: Application to a comparative pharmacokinetics study

Cited by 19 publications

References 35 publications

Incorporation of concentration data below the limit of quantification in population pharmacokinetic analyses

Incorporation of concentration data below the limit of quantification in population pharmacokinetic analyses

In vivo D2O labeling to quantify static and dynamic changes in cholesterol and cholesterol esters by high resolution LC/MS

Bioequivalence of Two Oral Contraceptive Drugs Containing Ethinylestradiol and Gestodene in Healthy Female Volunteers

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