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Comparison of extraction procedures for assessment of matrix effect for selective and reliable determination of atazanavir in human plasma by LC-ESI-MS/MS.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Feb 15; 885-886:138-49.JC

Abstract

A comparative study with three conventional extraction techniques namely protein precipitation (PP), liquid-liquid extraction (LLE) and solid phase extraction (SPE) has been demonstrated to assess the magnitude of matrix interference by post-column analyte infusion and post extraction analyte spiking for the determination of atazanavir from human plasma. Severe ion suppression observed in PP and to a lesser extent in LLE was circumvented by SPE on LiChrosep Sequence extraction cartridge. Based on these observations a selective, rugged and high throughput SPE-LC-MS/MS method has been developed for reliable determination of atazanavir in human plasma. The chromatographic separation was achieved on a Hypersil Gold C18 (50mm×4.6mm, 5μm) analytical column using 5mM ammonium formate in water:methanol (10:90, v/v) as the mobile phase under isocratic conditions. The method was validated over a wide dynamic concentration range of 10-6000ng/mL. The mean relative recovery and absolute matrix effect across quality controls were 84.9 and 93.2%, respectively. The precision value for relative matrix effect between eight different lots of plasma, expressed as %CV of the slopes of the calibration lines was 2.41. The stability of atazanavir under different storage conditions varied from -8.4 to 5.4%. The method was successfully applied to a bioequivalence study of 300mg atazanavir capsule formulation in 24 healthy Indian males under fasting condition.

Authors+Show Affiliations

Bioanalytical Research, CRO, Cadila Pharmaceuticals Ltd., Ahmedabad 387810, India; Chemistry Department, School of Sciences, KSKV Kachchh University, Bhuj 370001, India.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Randomized Controlled Trial

Language

eng

PubMed ID

22265353

Citation

Yadav, Manish, et al. "Comparison of Extraction Procedures for Assessment of Matrix Effect for Selective and Reliable Determination of Atazanavir in Human Plasma By LC-ESI-MS/MS." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 885-886, 2012, pp. 138-49.
Yadav M, Trivedi V, Upadhyay V, et al. Comparison of extraction procedures for assessment of matrix effect for selective and reliable determination of atazanavir in human plasma by LC-ESI-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2012;885-886:138-49.
Yadav, M., Trivedi, V., Upadhyay, V., Shah, G., Baxi, G. A., Goswami, S., & Shrivastav, P. S. (2012). Comparison of extraction procedures for assessment of matrix effect for selective and reliable determination of atazanavir in human plasma by LC-ESI-MS/MS. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 885-886, 138-49. https://doi.org/10.1016/j.jchromb.2011.12.031
Yadav M, et al. Comparison of Extraction Procedures for Assessment of Matrix Effect for Selective and Reliable Determination of Atazanavir in Human Plasma By LC-ESI-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Feb 15;885-886:138-49. PubMed PMID: 22265353.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Comparison of extraction procedures for assessment of matrix effect for selective and reliable determination of atazanavir in human plasma by LC-ESI-MS/MS. AU - Yadav,Manish, AU - Trivedi,Vikas, AU - Upadhyay,Vivek, AU - Shah,Gaurang, AU - Baxi,Girin A, AU - Goswami,Sailendra, AU - Shrivastav,Pranav S, Y1 - 2012/01/09/ PY - 2011/09/08/received PY - 2011/12/27/revised PY - 2011/12/28/accepted PY - 2012/1/24/entrez PY - 2012/1/24/pubmed PY - 2012/5/5/medline SP - 138 EP - 49 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 885-886 N2 - A comparative study with three conventional extraction techniques namely protein precipitation (PP), liquid-liquid extraction (LLE) and solid phase extraction (SPE) has been demonstrated to assess the magnitude of matrix interference by post-column analyte infusion and post extraction analyte spiking for the determination of atazanavir from human plasma. Severe ion suppression observed in PP and to a lesser extent in LLE was circumvented by SPE on LiChrosep Sequence extraction cartridge. Based on these observations a selective, rugged and high throughput SPE-LC-MS/MS method has been developed for reliable determination of atazanavir in human plasma. The chromatographic separation was achieved on a Hypersil Gold C18 (50mm×4.6mm, 5μm) analytical column using 5mM ammonium formate in water:methanol (10:90, v/v) as the mobile phase under isocratic conditions. The method was validated over a wide dynamic concentration range of 10-6000ng/mL. The mean relative recovery and absolute matrix effect across quality controls were 84.9 and 93.2%, respectively. The precision value for relative matrix effect between eight different lots of plasma, expressed as %CV of the slopes of the calibration lines was 2.41. The stability of atazanavir under different storage conditions varied from -8.4 to 5.4%. The method was successfully applied to a bioequivalence study of 300mg atazanavir capsule formulation in 24 healthy Indian males under fasting condition. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/22265353/Comparison_of_extraction_procedures_for_assessment_of_matrix_effect_for_selective_and_reliable_determination_of_atazanavir_in_human_plasma_by_LC_ESI_MS/MS_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(12)00018-9 DB - PRIME DP - Unbound Medicine ER -