Liquid chromatographic–tandem mass spectrometric assay for the simultaneous determination of didanosine and stavudine in human plasma, bronchoalveolar lavage fluid, alveolar cells, peripheral blood mononuclear cells, seminal plasma, cerebrospinal fluid and tonsil tissue

Huang, Yong; Zurlinden, Elisabeth; Lin, Emil T.; Li, Xiaohua; Tokumoto, Jason; Golden, Jeff; Murr, Andrew H.; Engstrom, John W.; Conte, John E.

doi:10.1016/j.jchromb.2003.10.043

Cited by 40 publications

(25 citation statements)

References 18 publications

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“…Cocktails of three to four drugs are used routinely in anti-HIV therapy [7]. Therefore, several analytical methods have been published for the simultaneous analysis of didanosine and other antiretroviral drugs in formulations and biological samples [2,[6][7][8][9][10][11][12][13]. Analytical methods for the quantitation of the active metabolite ddATP were developed using CE-MS and LC-MS/MS [3,14].…”

Section: Introductionmentioning

confidence: 99%

Method development and validation for the analysis of didanosine using micellar electrokinetic capillary chromatography

et al. 2005

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A selective MEKC method was developed for the analysis of didanosine in bulk samples. Successful separation of didanosine from 13 of its potential impurities, derived from the various synthetic preparation procedures, was achieved. As CZE gave poor separation selectivity, MEKC was preferable. The use of EKC allowed achievement of the separation in a significantly shorter time than conventional HPLC. An anionic long-chain surfactant, lithium dodecyl sulfate (LiDS), was used as the pseudostationary phase and sodium tetraborate buffer as the aqueous phase. In order to obtain the optimal conditions and to test the method robustness, a central composite response surface modeling experiment was performed. The optimized electrophoretic conditions include the use of an uncoated fused-silica capillary with a total length of 40 cm and an ID of 50 microm, a BGE containing 40 mM sodium tetraborate and 110 mM LiDS at pH 8.0, an applied voltage of 18.0 kV, and the capillary temperature maintained at 15 degrees C. The method was found to be robust. The parameters for validation such as linearity, precision, and sensitivity are also reported. Three commercial bulk samples were analyzed with this system.

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Section: Introductionmentioning

confidence: 99%

Method development and validation for the analysis of didanosine using micellar electrokinetic capillary chromatography

et al. 2005

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“…Samples for the determination of stavudine and its metabolites were isolated and purified by solid-phase extraction [47 -50] and deproteinated with a mixture of 2-propanol and dichloromethane (1 : 19) [51]. The analyses were performed with UV [50 -52) and mass-spectrometric detectors [47,48]. The lat- [28] ter ensure a detection threshold of 2 ng/ml [47] and 4 ng/ml [48] in the blood plasma and less than 0.5 ng/ml in other biological fluids (CSF, alveolar cells, peripheral mononucleated cells, bronchoalveolar fluid, tonsillar tissue) [47].…”

Section: Thymidine Derivativesmentioning

confidence: 99%

HPLC in biopharmaceutical investigations of drugs representing pyrimidine derivatives (A review)

et al. 2007

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Pyrimidine derivatives are widely used for the treatment of viral diseases and cancer. The analysis of pyrimidine derivatives is typically performed using various chromatographic techniques, in particular, reversed-phase high performance liquid chromatography (HPLC). The separation is typically carried out with (7 -30)-cm-long C 8 and C 18 silica gel columns, mainly at room temperature, and a 1 -1.5 ml/min eluent flow rate. The column is eluted in an isocratic or gradient system, and a variety of mobile phases have been proposed. The detection is based on optical absorption or fluorescence measurements, or makes use of mass spectrometry. Various methods of extraction of pyrimidine derivatives from biological samples are discussed, and the corresponding detection limits are presented.

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“…Comparable results indicate lack of matrix effects or inconsistent matrix effects but this approach does not positively identify the magnitude of the matrix effects. Huang et al used LC-UV to detect the down-field matrix peaks that caused ion suppression for the analyte of interest and modified the chromatographic condition [113]. Another approach for assessing consistent matrix effect among the individual matrix lots is to measure the consistency for the results obtained from sample from individual matrix lot (typically n > 6) [114][115][116][117][118][119][120][121][122][123].…”

Section: Matrix Effects and Recoverymentioning

confidence: 99%

Critical Review of Development, Validation, and Transfer for High Throughput Bioanalytical LC-MS/MS Methods

Zhou¹,

Song²,

Tang³

et al. 2005

CPA

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Swift growth in the use of LC-MS/MS for the analysis of drugs in biological matrices has been compelled by the need for timely and high-quality data at many stages in drug discovery and development process: from high throughput screening of drug candidates and rapid data generation for pre-clinical studies to almost 'real-time' analysis of clinical samples. Prompt and rational method development, validation, and transfer play a pivotal role in achieving the goals of "faster, better, and cheaper" for pharmacokinetic studies since this could easily account for more than 50% of the time and labor resources for a moderate-sized project. Strategy for rational method development, validation and transfer has been largely kept as institutional knowledge but rarely appeared in literature. In this review article, strategies for developing and validating robust high throughput LC-MS/MS methods will be critically reviewed and discussed. Automated sample preparation, fast chromatography, minimization of matrix effects, and strategy of narrowing the gap between validation and incurred sample analysis are just a few topics covered in this review. Other interesting approaches for improving method efficiency and ruggedness such as direct injection SPE and liquid/liquid extracts as well as multiplexing of LC columns will also be discussed. Potential pitfalls during method development and validation are pointed out. At the end, the question "how fast is fast enough and how fast is too fast?" will be answered after considering all aspects of the method development and validation.

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Liquid chromatographic–tandem mass spectrometric assay for the simultaneous determination of didanosine and stavudine in human plasma, bronchoalveolar lavage fluid, alveolar cells, peripheral blood mononuclear cells, seminal plasma, cerebrospinal fluid and tonsil tissue

Cited by 40 publications

References 18 publications

Method development and validation for the analysis of didanosine using micellar electrokinetic capillary chromatography

Method development and validation for the analysis of didanosine using micellar electrokinetic capillary chromatography

HPLC in biopharmaceutical investigations of drugs representing pyrimidine derivatives (A review)

Critical Review of Development, Validation, and Transfer for High Throughput Bioanalytical LC-MS/MS Methods

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