Validation of liquid chromatographic and gas chromatographic methods Applications to pharmacokinetics

Bressolle, Françoise; Bromet-Petit, Maguy; Audran, Michel

doi:10.1016/s0378-4347(96)00088-6

Cited by 384 publications

(265 citation statements)

References 11 publications

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“…The guiding principles [41][42][43][44][45][46][47][48][49][50][51][52][53][54][55][56][57] for validation of bioanalytical methods were used as references to design the experiments. Since PGs, DiHETrEs, HETEs, EETs, and AA are endogenous compounds, the analyte-free brain matrix is not available for matrix-based method validation and there is no other proxy matrix available to mimic the complicated solid brain tissue.…”

Section: Methods Validation Design-mentioning

confidence: 99%

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

Yue

Jansen

Strauss

et al. 2007

Journal of Pharmaceutical and Biomedical Analysis

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A sensitive, specific, and robust liquid chromatography/mass spectrometric (LC/ MS) method was developed and validated that allows simultaneous analysis of arachidonic acid (AA) and its cyclooxygenase, cytochrome P450, and lipoxygenase pathway metabolites prostaglandins (PGs), dihydroxyeicosatrienoic acids (DiHETrEs), hydroxyeicosatetraenoic acids (HETEs) and epoxyeicosatrienoic acids (EETs), including PGF 2α , PGE 2 , PGD 2 , PGJ 2 ,14,11,8,5,14,11,8,9-EET, and 5,6-EET in rat brain tissues. Deuterium labeled PGF 2α -d 4 , PGD 2 -d 4 , 15(S)-HETE-d 8 , 14,15-EET-d 8 , 11,12-EET-d 8 , 8,9-EET-d 8 , and AA-d 8 were used as internal standards. Solid phase extraction was used for sample preparation. A gradient LC/MS method using a C18 column and electrospray ionization source under negative ion mode was optimized for the best sensitivity and separation within 35 min. The method validation, including LC/MS instrument qualification, specificity, calibration model, accuracy, precision (without brain matrix and with brain matrix), and extraction efficiency were performed. The linear ranges of the calibration curves were 2-1000 pg for PGs, DiHETrEs, HETEs, and EETs, 10-2400 pg for PGE 2 and PGD 2 , and 20-2000 ng for AA, respectively.

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Section: Methods Validation Design-mentioning

confidence: 99%

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

Yue

Jansen

Strauss

et al. 2007

Journal of Pharmaceutical and Biomedical Analysis

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“…After a solid-phase extraction procedure, compounds were identified and quantified by liquid chromatography͞electrospray ionization MS (LC͞ESI-MS) and validated according to U.S. Food and Drug Administration Good Laborator y Practices guidelines (17,18).…”

Section: Methodsmentioning

confidence: 99%

Prodrugs of bisthiazolium salts are orally potent antimalarials

Vial

Wein

Farenc

et al. 2004

Proc. Natl. Acad. Sci. U.S.A.

105

151

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We created neutral antimalarial prodrugs that deliver bisthiazolium compounds with antimalarial activity in the nanomolar range. These drugs primarily affect early intraerythrocytic stages through rapid, nonreversible cytotoxicity. The compounds are suitable for both parenteral and oral use and plasma promotes rapid conversion of the prodrug into the drug. We demonstrate that very low doses offer protection in a murine model of malaria. The drugs show great potential for curing high parasitemia with short-course treatments. Oral administration of the TE3 prodrug completely cures Plasmodium cynomolgi infection in rhesus monkeys. The drugs specifically accumulate inside infected erythrocytes, block phosphatidylcholine biosynthesis, and interact with hemozoin. To our knowledge, this class of compounds represents one of the most potent antimalarials tested to date. These unique properties signal a promising future for this class of antimalarial.M alaria is a public health problem affecting Ͼ40% of the world's population. It causes up to 2 million deaths, mostly young children, in Africa, and Ͼ300 million clinical cases each year (1), with major consequent impact on economic productivity and livelihood (2). Currently, there are no licensed vaccines and the spread of drug-resistant parasites and insecticideresistant mosquitoes is an increasing problem. New antimalarial compounds, particularly those based on compounds structurally unrelated to existing antimalarial drugs with new mechanisms of action, are urgently needed (3-5).We have developed classes of antimalarial drugs targeting membrane biogenesis during intraerythrocytic Plasmodium falciparum development. We have focused on mono-and bisquaternary ammonium compounds for their potent antimalarial activity in vitro and in vivo (6, 7). These compounds mimic choline structure; they potently inhibit the low-affinity choline carrier related to phospholipid biosynthesis in eukaryotic cells and the high-affinity carrier involved in biosynthesis of the neurotransmitter acetylcholine in the CNS (8, 9). These compounds have exceptional in vitro and in vivo antimalarial properties devoid of mutagenic activity (10 -12).G25 [1,16-hexadecamethylenebis(N-methylpyrrolidinium) dibromide] and other drugs in this class possess a permanently charged cationic group (7, 13) that is essential for activity but detrimental to oral absorption. This action prejudiced development for the clinic. Oral administration is essential for treatment in dispensaries in endemic countries and for prophylactic or curative treatment for travelers. A targeting carrier system is unsuitable because, in the absence of carrier-mediated specific processes, quaternary ammonium compounds are intrinsically incapable of crossing bilayered cellular membranes. Designing drugs that mask the ionizable groups was therefore the most attractive solution. This was the rationale behind development of a chemically modified form of drug that is converted into an active ionized form by enzymes present in plasma. Here, we repo...

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“…4); the mean matrix factors ranged from 88 to 101% in human plasma (CVs, 7 -9%), and from 93 to 101% in rat plasma (CVs, 6.0 -7.0%). Precision and accuracy values were within acceptable limits ( [18,21], US Food and Drug Administration. Guidance for industry.…”

Section: Validationmentioning

confidence: 82%

“…The retention times of EAPB0503, EAPB0603 and internal standard were 6.7, 4.5, and 8.6 min, respectively (CVs, 1.0 -2.3%, n = 30). For both EAPB0503 and EAPB0603, quadratic calibration curves gave the best fit based on the statistical analysis results [21] and precision and recovery of QC samples. CV values on the slope b were a 30% in human and rat plasma (Table 1).…”

Section: Mass Spectra and Chromatographymentioning

confidence: 98%

Quantitation of imidazo[1,2‐a]quinoxaline derivatives in human and rat plasma using LC/ESI‐MS

Khier

Moarbess²,

Deleuze‐Masquéfa³

et al. 2009

J of Separation Science

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Original PaperQuantitation of imidazo[1,2-a]quinoxaline derivatives in human and rat plasma using LC/ESI-MS Since several years, our group developed quinoxalinic compounds. Among the synthesized compounds, in the imidazo[1,2-a]quinoxaline series, EAPB0203 has shown interesting activities both on melanoma and lymphoma. The structure of EAPB0203 has been modulated and a new compound, EAPB0503, exhibits an in vitro cytotoxic activity on melanoma cancer cell line 7 -9 times higher than EAPB0203. We validated an LC/ESI-MS method to simultaneously quantify EAPB0503 and its metabolite EAPB0603 in human and rat plasma. Chromatography was performed on a C8 Zorbax eclipse XDB column with a mobile phase consisting of acetronitrile and formate buffer gradient elution. LC-MS data were acquired in SIM mode at m/z 305, 291, and 303 for EAPB0503, EAPB0603, and the internal standard, respectively. The drug/ internal standard peak area ratios were linked via quadratic relationships to concentrations (low range: 5 -300 lg/L, high range: 100 -1000 lg/L). The method is precise (precision, f14%) and accurate (recovery, 92 -113%). Mean extraction efficiencies, A72% for each analyte, were obtained. The lower LOQs were 5 lg/L. This highly specific and sensitive method was successfully used to investigate plasma concentrations of EAPB0503 and EAPB0603 in a pharmacokinetic study carried out in rat and would also be useful in clinical trials at a later stage.Keywords: Human and rat matrices / Imidazo[1,2-a]quinoxaline / LC/ESI-MS / Lymphoma / Melanoma /

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Validation of liquid chromatographic and gas chromatographic methods Applications to pharmacokinetics

Cited by 384 publications

References 11 publications

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

Prodrugs of bisthiazolium salts are orally potent antimalarials

Quantitation of imidazo[1,2‐a]quinoxaline derivatives in human and rat plasma using LC/ESI‐MS

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