Development and validation of an HPLC–MS/MS method to determine clopidogrel in human plasma. Use of incurred samples to test back-conversion

Silvestro, Luigi; Gheorghe, Mihaela; Tarcomnicu, Isabela; Savu, S N; Savu, Simona Rizea; Iordăchescu, A.; Dulea, Constanta

doi:10.1016/j.jchromb.2010.09.022

Cited by 37 publications

(25 citation statements)

References 12 publications

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“…there is no concern associated with AG) appear to assume that an interfering metabolite, if present, is moderately stable, because a typical reference value is established from a sample that is collected without special care, shipped in a frozen state, and measured at a bioanalytical laboratory. A number of case studies typically determined frozen long-term stability [18][19][20][21][22][23][24][25][26], some of which also examined other test items. Test items and study design were surveyed by EBF [27] and GCC [7] and extensively discussed by Yadav et al [28].…”

Section: Discussionmentioning

confidence: 99%

Incurred sample stability of ASP3258 in the presence of its acyl glucuronide

Ohtsu¹

2017

J Appl Bioanal

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The acyl glucuronide (AG) of ASP3258 was abundant in incurred monkey samples, and because an AG generally back-converts to its aglycone, accurate quantification of ASP3258 in monkey plasma was a challenge. To prevent the back-conversion of ASP3258-AG, cooling and acidification were incorporated during sample collection, storage, and extraction. To demonstrate that the AG did not affect the determination of ASP3258, the present study used incurred samples to examine whole blood stability, short-term stability, freeze-thaw stability, frozen stability, and stability during extraction. The concentration changes were within −11.4% to 15.0% compared with a reference value and were therefore judged acceptable. The present study presents a detailed account of test items, a reference value, sample numbers, sample selection, and an equation for assessment in the incurred sample stability tests. This bioanalytical method was applied successfully to a study of the toxicokinetics of ASP3258 in monkeys.Keywords: incurred sample stability, acyl glucuronide, ASP3258, animal plasma, toxicokinetics. IntroductionThe potent phosphodiesterase 4 inhibitor ASP3258 (Figure 1) is a novel therapeutic agent for asthma and chronic obstructive pulmonary disease [1]. We previously developed and validated a bioanalytical method to quantify ASP3258 in rat plasma [2]. Because ASP3258 metabolite was not detected in rat plasma [3], this bioanalytical method was developed without encountering issues associated with the metabolite. Subsequently, monkey toxicity studies were planned that required an appropriate bioanalytical method. When ASP3258 was orally administered to monkeys in a preliminary study, the acyl glucuronide (AG) metabolite of ASP3258 was detected in abundance in monkey plasma (data on file), in contrast to our findings using rat plasma [3]. In general, AGs readily back-convert to aglycones, causing overestimation of

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Section: Discussionmentioning

confidence: 99%

Incurred sample stability of ASP3258 in the presence of its acyl glucuronide

Ohtsu¹

2017

J Appl Bioanal

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“…The drug is an irreversible inhibitor of the P2Y12 adenosine diphosphate receptor found on the membranes of platelet cells. Clopidogrel specifically and irreversibly inhibits the P2Y12 subtype of ADP receptor, which is important in aggregation of platelets and cross-linking by the protein fibrin.Various analytical methods involving HPLC [18,19], LC-MS [20] and LC-MS/MS [21] have been reported for the analysis of clopidogrel. To date, no HPLC method is available for the simultaneous estimation of pioglitazone, amlodipine, atorvastatin and clopidogrel in tablet dosage form, which prompted to pursue the present work.…”

Section: Pioglitazone (P) Is 5-[[4-[2-(methyl-2-pyridinylamino)-ethoxmentioning

confidence: 99%

Synchronised Separation of Antihypertensive, Antidiabetic and Antihyperlipidemic Drugs by RP-HPLC

Monika¹,

Chawla²,

Pandey³

2017

Asian J. Chem.

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A new simple, rapid and precise reverse phase isocratic HPLC method has been developed for estimation of pioglitazone, amlodipine, atorvastatin and clopidogrel simultaneously. The separation was achieved on a Millenium M-Sil C18 (125 mm × 4.6 mm) column using a mobile phase comprising of methanol:0.02 M KH2PO4 (65:35) and pH adjusted 4.5 with 0.01 % orthophosphoric acid. Stocks and dilutions were prepared in mobile phase. The flow rate was kept at 1 mL/min and analytes were screened with a UV detector. The retention time of pioglitazone, amlodipine, atorvastatin and clopidogrel were 3.17, 4.05, 6.09 and 13.73 min, respectively. The method was validated according to ICH guidelines with respect to linearity, accuracy, precision and specificity. The linearity range was found to be 0.625 to10 µg/mL for all drugs. The limit of detection of pioglitazone, amlodipine, atorvastatin and clopidogrel were 0.11, 0.03, 0.048 and 0.14, respectively and limit of quantitation were 0.34, 0.10, 0.14 and 0.43 µg/mL. The method was validated as a final confirmation of method development with respect to its linearity, precision, accuracy, ruggedness and robustness. This validated method can be handy for the evaluation of various commercially available pharmaceutical dosage forms with high precision and reproducibility.

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“…Shell particles are a relatively recent trend in chromatographic separation, but several pharmaceutical-bioanalytical [105][106][107][108][109][110][111][112][113][114][115][116][117][118], food analytical [119][120][121][122][123][124][125][126][127][128][129], environmental [130][131][132][133][134] and multidimensional [135][136][137] separations can be found in the literature. Very recently, new commercially available wide-pore stationary phases demonstrate exceptional efficiency for protein separations [138][139][140].…”

Section: Superficially Porous Particlesmentioning

confidence: 99%

Evolution and Current Trends in Liquid and Supercritical Fluid Chromatography

Fekete¹,

Perrenoud²,

Guillarme

2014

CCHG

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Abstract:The current trend in high performance liquid chromatography (HPLC) tends toward the achievement of higher separation efficiency and shorter analysis time. Indeed, better performance in LC has become increasingly important in recent years mainly driven by the challenges of either analyzing more complex samples or increasing the numbers of samples per time unit. In the recent development of particle technology, the use of fully porous sub-2 m particles and sub-3 m shell particles have received considerable attention. Beside packed columns, the new generation of silica-based monolithic columns also offers very high separation power. However, to take full advantage of these innovative phases, the chromatographic system has also to be drastically optimized in terms of upper pressure limit and system volume.This revolution in column technology now spreads and covers several modes of liquid chromatography such as reversedphase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC), or even supercritical fluid chromatography (SFC). The HILIC and SFC, which can be considered as alternative modes of chromatography, could also be useful to extend the applicability of chromatography towards the analysis of very hydrophilic and lipophilic compounds, respectively.The present review gives an insight about the theory behind the success of current column technology and presents a summary of latest applications, using various modes of one-dimensional chromatography (RPLC, HILIC, SFC). This paper also shows that theoretically expected column efficiency could sometimes be compromised in practical work especially in the case of narrow bore columns.

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Development and validation of an HPLC–MS/MS method to determine clopidogrel in human plasma. Use of incurred samples to test back-conversion

Cited by 37 publications

References 12 publications

Incurred sample stability of ASP3258 in the presence of its acyl glucuronide

Incurred sample stability of ASP3258 in the presence of its acyl glucuronide

Synchronised Separation of Antihypertensive, Antidiabetic and Antihyperlipidemic Drugs by RP-HPLC

Evolution and Current Trends in Liquid and Supercritical Fluid Chromatography

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