A simple and sensitive high performance liquid chromatography assay with a fluorescence detector for determination of canagliflozin in human plasma

2015 ◽  
Vol 7 (7) ◽  
pp. 3028-3035 ◽  
Author(s):  
Muzaffar Iqbal ◽  
Nasr Y. Khalil ◽  
Amer M. Alanazi ◽  
Khalid A. Al-Rashood

Simple and sensitive HPLC assay for accurate quantification of canagliflozin in human plasma using telmisartan as the internal standard.

2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.


2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
John Teye Azietaku ◽  
Xie-an Yu ◽  
Jin Li ◽  
Jia Hao ◽  
Jun Cao ◽  
...  

A specific, sensitive, and reliable high performance liquid chromatography with fluorescence detection (HPLC-FLD) was first optimized and then used in the simultaneous quantification of bergapten, imperatorin, notopterol, and isoimperatorin in rat plasma using osthole as the internal standard. Liquid-liquid extraction with ethyl acetate was employed in treating the rat plasma samples obtained. Separation was carried out with a Hedera™ ODS column (4.6 × 250 mm, 5 μm) by gradient elution at a temperature of 40°C. Excitation and emission of the fluorescence detector were set to 300 and 490 nm, respectively. The lower limits of quantification for bergapten, imperatorin, notopterol, and isoimperatorin in rat plasma were 4, 40, 4, and 2 ng mL−1, respectively. The intraday and interday precision and accuracy for the four coumarins were within acceptable criteria. The recovery of the method was satisfactory with a range of 80.3–114%. The validated method was successfully used for the simultaneous determination of the four coumarins in Notopterygium incisum extracts and also for the pharmacokinetic and excretion study of bergapten, imperatorin, notopterol, and isoimperatorin in rats.


1995 ◽  
Vol 14 (1) ◽  
pp. 34-37 ◽  
Author(s):  
A. Belmadani ◽  
I. Combourieu ◽  
M. Bonini ◽  
E.E. Creppy

Fluvoxamine is an antidepressant drug introduced into the clinic in 1986. It acts by selectively inhibiting neuronal serotonin recapture. It can be quantified by several meth ods, including high performance liquid chromatography. The HPLC method used so far needs special equipment and has poor sensitivity. The technique is difficult and time consuming. An easier, quicker and more sensitive HPLC assay for the routine determination of fluvoxamine in human plasma has therefore been developed. After alkalinisation and direct extraction by a mixture of n-hexane-isoamylic alcohol 985: 15 (v/v) of plasma samples, the organic phases were further extracted by HCl 0.1 N. Thirty μL of the final extract (with loxapine as internal standard) were injected directly into a C-8 column with a mobile phase consisting of 370 mL acetonitrile, 0.4 mL diethylamine, 630 mL of distilled water, 25 mL pic B5. UV detection at 254 nm was used. The whole process was completed in 40 min. The detec tion limit was 10 ng mL-1. No interference was found either with several benzodiazepines or with antidepres sant drugs commonly associated during treatments.


2013 ◽  
Vol 781-784 ◽  
pp. 903-907
Author(s):  
Dong Mei Huang ◽  
Jie Xu ◽  
Yong Fu Shi ◽  
Xuan Yun Huang ◽  
Huan Yu ◽  
...  

The method was established to detect fourteen sulfonamides residuces in Penaeus vannamei by high performance liquid chromatography coupled with post-column derivation. Sulfonamides residues were extracted with ethyl acetate after adding sulfapyridine as internal standard. The extract was concentrated.The residues were transferred to hydrochloric acid solution. The solution was defatted with n-hexane. The compounds were detected by HPLC with fluorescence detector .The standard addition method was used. The calibration curves were linear. The recoveries ranged from 77.8% to 103.6%. The relative standard deviations were all below 9.1%. Quantitative detection limits of fourteen sulfanomides ranged from1.0μg/kg to 5.0μg/kg. Results indicated that the method was easier, faster and more accurate.


2016 ◽  
Vol 60 (8) ◽  
pp. 4734-4742 ◽  
Author(s):  
Tiphaine Legrand ◽  
Dominique Vodovar ◽  
Nicolas Tournier ◽  
Nihel Khoudour ◽  
Anne Hulin

ABSTRACTA simple and rapid ultra-high-performance liquid chromatography (UHPLC) method using UV detection was developed for the simultaneous determination of eight β-lactam antibiotics in human plasma, including four penicillins, amoxicillin (AMX), cloxacillin (CLX), oxacillin (OXA), and piperacillin (PIP), and four cephalosporins, cefazolin (CFZ), cefepime (FEP), cefotaxime (CTX), and ceftazidime (CAZ). One hundred-microliter samples were spiked with thiopental as an internal standard, and proteins were precipitated by acetonitrile containing 0.1% formic acid. Separation was achieved on a pentafluorophenyl (PFP) column with a mobile phase composed of phosphoric acid (10 mM) and acetonitrile in gradient elution mode at a flow rate of 500 μl/min. Detection was performed at 230 nm for AMX, CLX, OXA, and PIP and 260 nm for CFZ, FEP, CTX, and CAZ. The total analysis time did not exceed 13 min. The method was found to be linear at concentrations ranging from 2 to 100 mg/liter for each compound, and all validation parameters fulfilled international requirements. Between- and within-run accuracy errors ranged from −5.2% to 11.4%, and precision was lower than 14.2%. This simple method requires small-volume samples and can easily be implemented in most clinical laboratories to promote the therapeutic drug monitoring of β-lactam antibiotics. The simultaneous determination of several antibiotics considerably reduces the time to results for clinicians, which may improve treatment efficiency, especially in critically ill patients.


2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.


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