Rapid analysis of benzodiazepines in whole blood by high-performance liquid chromatography: use of a monolithic column

Bugey, Aurélie; Staub, Christian

doi:10.1016/j.jpba.2004.01.023

Cited by 78 publications

(60 citation statements)

References 30 publications

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“…These methods include spectrophotometry and spectrofluorimetry [2][3][4], potentiometry [5,6], indirect kinetic catalytic method by stopped flow technique [7], immunoassays [8], modified carbon-paste electrodes as sensors [9], but the vast majority of the published methods involve separation techniques, particularly HPLC [10][11][12][13][14][15][16], MEKC [17][18][19], LC-MS [20][21][22][23][24], with atmospheric pressure chemical ionization [25], ESI [26][27][28][29], thermospray ionization [30], negative ion chemical ionization [31], GC [32][33][34][35][36][37][38], GC-MS [39][40][41], and CE [28,42].…”

Section: Introductionmentioning

confidence: 99%

Development of a validated HPLC method for the determination of four 1,4‐benzodiazepines in human biological fluids

Samanidou

Pechlivanidou

Papadoyannis³

2007

J of Separation Science

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A simple and sensitive HPLC method was developed and validated for the determination of four frequently prescribed 1,4-benzodiazepines: alprazolam (ALP), bromazepam (BRZ), diazepam (DZP), and flunitrazepam (FNZ). Separation was achieved on an Inertsil C8 analytical (250 mm x 4 mm, 5 microm) column, after selective extraction of benzodiazepine drugs from biological matrices by means of SPE. Isocratic elution was performed with a mobile phase consisting of CH3COONH4, 0.05 M CH3OH, and CH3CN (33:57:10 by volume). Quantification was performed at 240 nm with mefenamic acid (6 ng/microL) as the internal standard. DSC-18 Supelco cartridges provided high absolute recoveries (81-115%). The developed method was fully validated in terms of selectivity, linearity, accuracy, precision, stability, and sensitivity. Repeatability (n = 8) and between-day precision (n = 8) revealed RSD <12%. Recoveries from biological samples ranged from 81.2 to 115%. The detection limit of the method was calculated as 3.3-10.2 ng in blood plasma and 2.6-12.6 ng in urine for 20 microL injection volume. The method was applied to spiked biological matrices. Moreover, the method was applied to real samples of urine after an oral administration.

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Section: Introductionmentioning

confidence: 99%

Development of a validated HPLC method for the determination of four 1,4‐benzodiazepines in human biological fluids

Samanidou

Pechlivanidou

Papadoyannis³

2007

J of Separation Science

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“…Chromolith (25 Â 4.6 mm) [34], Chromolith SpeedRod RP-18 (50 Â 4.6 mm) [35] Furosemide [30,31], norfloxacin [31] [ 30,31] Sotalol [32] Losartan [33,34], telmisartan [34], valsartan [34] [ 33,34] Verapamil, indiplon [35] Drugs of abuse CEC [36], FIA/HPLC-CID [37], HPLCfluorescence [38,39], HPLC-DAD [40] Urine [36,37,39], plasma [38,39], saliva [39], whole blood [40], solvent [37] Described in text [36], Chromolith Flash RP-18e (25 Â 4.6 mm) [37], Chromolith Performance RP-18e (50 Â 4.6 mm) [38], (100 Â 4.6 mm) [39,40] 3,4-Methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, 4-hydroxy-…”

Section: Hplc-ms/ms [21]mentioning

confidence: 99%

“…The linear range is up to 2.1 mmol/L (500 ng/mL) in plasma, up to 25.49 mmol/L (6000 ng/mL) in saliva, and up to 0.42 mmol/L (100 mg/mL) in urine. Measuring eight benzodiazepines (o4.0 min) in whole blood using HPLC-UV at 220 nm was reported with an LOQ of 0.06 mmol/L (20 ng/mL) for clonazepam, desalkylflurazepam, flunitrazepam, lorazepam, and midazolam and 0.1 mmol/L (30 ng/mL) for diazepam, nordiazepam, and oxazepam [40]. The assay is linear up to 1.60 mmol/L (500 ng/mL) for clonazepam, desalkylflurazepam, flunitrazepam, lorazepam, and midazolam and up to 18.47 mmol/L (5000 ng/mL) for diazepam, nordiazepam, and oxazepam, with a CV o7% for all analytes.…”

Section: Drugs Of Abusementioning

confidence: 99%

Applications of monolithic columns in liquid chromatography‐based clinical chemistry assays

Bunch

Wang

2011

J of Separation Science

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Monolithic columns have slowly been applied to HPLC methods for clinical chemistry testing in the last 10 years. The application areas include therapeutic drug monitoring, drugs of abuse, vitamins, porphyrins, and steroids. In comparison with conventional particulate columns, the monolithic columns may offer shorter chromatography time, more robustness, and better resolution for certain analytes. The potential drawback of large mobile phase consumption may be improved with smaller id columns, which are currently on the market. Methods covered in this review are those searchable in PubMed up to December 2010. This review highlights the emergence of monolithic column technology in HPLC methods used for clinical chemistry testing. The goals of this review are threefold: (i) To identify the areas of clinical chemistry that analytical monolithic columns have been used in HPLC methods. (ii) To demonstrate the application of analytical monolithic columns in HPLC methods using different detection systems. (iii) To discuss the advantages and limitations of the monolithic columns compared with particulate columns in the clinical chemistry applications.

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“…Liquidliquid extraction [13], solid-phase extraction (SPE) [14][15][16], online SPE [17] and solid-phase microextraction [18] have usually been successfully employed. Different analytical methods have been effectively developed and established to both identify and quantify these compounds; relevant information on a selected number of BZD-based applications is presented in Table 1.…”

Section: Introductionmentioning

confidence: 99%

Experimental design for optimization of microwave-assisted extraction of benzodiazepines in human plasma

Fernández¹,

Vázquez²,

Lorenzo

et al. 2010

Anal Bioanal Chem

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A simple and fast microwave-assisted-extraction (MAE) method has been evaluated as an alternative to solid-phase extraction (SPE) for the determination of six benzodiazepines widely prescribed in European countries (alprazolam, bromazepam, diazepam, lorazepam, lormetazepam and tetrazepam) in human plasma. For MAE optimization a Doehlert experimental design was used with extraction time, temperature and solvent volume as influential parameters. A desirability function was employed in addition to the simultaneous optimization of the MAE conditions. The analysis of variance showed that the solvent volume had a positive influence on the extraction of all the analytes tested, achieving a statistically significant effect. Also, the extraction time had a statistically significant effect on the extraction of four benzodiazepines. The selected MAE conditions-89°C, 13 min and 8 mL of chloroform/2-propanol (4:1, v/v)-led to recoveries between 89.8±0.3 and 102.1±5.2% for benzodiazepines using a high performance liquid chromatography method coupled with diode-array detection. The comparison of MAE and SPE shows better results for MAE, with a lower number of steps in handling the sample and greater efficiency. The applicability of MAE was successfully tested in 27 plasma samples from benzodiazepine users.

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Rapid analysis of benzodiazepines in whole blood by high-performance liquid chromatography: use of a monolithic column

Cited by 78 publications

References 30 publications

Development of a validated HPLC method for the determination of four 1,4‐benzodiazepines in human biological fluids

Development of a validated HPLC method for the determination of four 1,4‐benzodiazepines in human biological fluids

Applications of monolithic columns in liquid chromatography‐based clinical chemistry assays

Experimental design for optimization of microwave-assisted extraction of benzodiazepines in human plasma

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