Simultaneous determination of eight β-lactam antibiotics in human serum by liquid chromatography–tandem mass spectrometry

Ohmori, Tomofumi; Suzuki, Akio; Niwa, Takashi; Ushikoshi, Hiroaki; Shirai, Kunihiro; Yoshida, Shozo; Ogura, Shinji; Itoh, Yoshinori

doi:10.1016/j.jchromb.2011.03.001

Cited by 111 publications

(92 citation statements)

References 32 publications

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“…Liquid chromatography tandem mass spectrometry (LCMSMS) methods have also been described [50][51][52][53].The use of mass spectroscopy detectors allows a more definitive identification and quantitative determination of compounds, even with low resolution chromatography; a future not possible with other methods of HPLC detection [54]. LCMSMS Page 9 of 48 A c c e p t e d M a n u s c r i p t 9 also offers short time of analysis and is generally regarded as superior to HPLC methods because risk of false positive results is minimal.…”

Section: Page 8 Of 48mentioning

confidence: 99%

“…Further to this, the existing simultaneous methods do not encompass all relevant antibiotics as far as TDM in critical care is concerned. For example the method by Ohmori et al [50] can analyse eight -lactams simultaneously. However this method does not include all commonly used drugs such as benzylpenicillin, ertapenem, ceftazidime and flucloxacillin which are of interest in -lactam TDM and included in the present method.…”

Section: Page 8 Of 48mentioning

confidence: 99%

“…The primary stocks were then diluted with water to give 5 mg/mL standard solutions for each antibiotic and were stored in 1 mL aliquots at -80 °C under which condition -lactams are known to be stable at least for few months [45,46,50,51]. These standard solutions were used to prepare fresh standards and QCs in plasma for every analytical run.…”

Section: Preparation Of Solutions Standards and Quality Control Sammentioning

confidence: 99%

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Simultaneous determination of seven β-lactam antibiotics in human plasma for therapeutic drug monitoring and pharmacokinetic studies

Sime

Roberts

et al. 2014

Journal of Chromatography B

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This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain. AbstractThere is strong evidence in literature supporting the benefit of monitoring plasma concentrations of -lactam antibiotics in the critically ill to ensure appropriateness of dosing.The objective of this work was to develop a method for the simultaneous determination of total concentrations piperacillin, benzylpenicillin, flucloxacillin, meropenem, ertapenem, cephazolin and ceftazidime in human plasma. Sample preparation involved protein precipitation with acetonitrile containing 0.1% formic acid and subsequent dilution of supernatant with 0.1% formic acid in water. Chromatographic separation was achieved on a reversed phase column (C18, 2.6µm, 2.1* 50 mm) via gradient elution using water and acetonitrile, each containing 0.1% formic acid, as mobile phase. Tandem mass spectrometry (MSMS) analysis was performed, after electrospray ionization in the positive mode, with multiple reaction monitoring (MRM). The method is accurate with the inter-day and intra-day accuracies of quality control samples (QCs) ranging from 95%-107% and 95%-108%, respectively. It is also precise with intra-day and inter-day coefficient of variations ranging from 4 to 12 % and 5-14% respectively. The lower limit of quantification was 0.1g/mL for each antibiotic except flucloxacillin (0.25g/mL). Recovery was greater than 96% for all analytes except for ertapenem (78%). Coefficients of variation for the matrix effect were less than 10% over the six batches of plasma. Analytes were stable over three freeze-thaw cycles, and for reasonable hours on the bench top as well as post-preparation. This novel liquid chromatography tandem mass spectrometry method proved accurate, precise and applicable for therapeutic drug monitoring and pharmacokinetic studies of the selected -lactam antibiotics.Page 5 Highlights  We present a method for simultaneous determination of seven beta-lactams in plasma  The selected antibiotics are those commonly used in critically ill patients  The method is accurate, precise and meets validation requirements by guidelines  It proved applicable for therapeutic drug monitoring and pharmacokinetic studies

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Section: Page 8 Of 48mentioning

confidence: 99%

Section: Page 8 Of 48mentioning

confidence: 99%

Section: Preparation Of Solutions Standards and Quality Control Sammentioning

confidence: 99%

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Simultaneous determination of seven β-lactam antibiotics in human plasma for therapeutic drug monitoring and pharmacokinetic studies

Sime

Roberts

et al. 2014

Journal of Chromatography B

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“…Specimens were centrifuged at 3000 rpm for 10 minutes within 30 minutes of sampling and frozen at −80°C. Determination of piperacillin in plasma samples was performed using the liquid chromatography-tandem mass spectrometry (LC-MS/MS) modified method [6]. Unbound concentrations were calculated using published studies on the fraction of protein binding for the study drug [7].Urine samples were taken from a 1−8 hour and 24-hour urine collection in order to calculate cumulative renal excretion of piperacillin and creatinine clearance (Cl cr ), respectively.…”

Section: Sampling and B-lactam Assaymentioning

confidence: 99%

pilot study on pharmacokinetic/pharmacodynamic target attainment in critically ill patients receiving piperacillin/tazobactam

Martı́nková¹,

Malbrain²,

Havel³

et al. 2016

Anaesthesiol Intensive Ther

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Background: In critically ill patients, multi-trauma and intensive therapy can influence the pharmacokinetics (PK) and pharmacodynamics (PD) of antibiotics with time-dependent bacterial killing. Consequently, PK/PD targets (%fT >MIC ) -crucial for antimicrobial effects -may not be attained. Methods: Two patients admitted to the surgical ICU of the University Hospital in Hradec Králove for multiple-trauma were given piperacillin/tazobactam by 1-hour IV infusion 4/0.5 g every 8 h. PK variables: total and renal clearance (CL tot , CL R ), volume of distribution (V d ), and elimination half-life (T 1/2 ) were calculated, followed by glomerular filtration rate (MDRD) and cumulative fluid balance (CFB-total fluid volume based on 24-h registered fluid intake minus output). The PK/PD target attainment (100%fT >MIC ) was defined as free (f) piperacillin plasma concentrations that remain, during the entire dosing interval (T), above the minimum inhibitory concentration (100%fT> MIC ) within days 4-8 (when CFB culminates and disappears). Piperacillin concentrations were determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and corrected for unbound fraction (22%). Results: CFB culminated over days 2−5 reaching 15−30 L and was associated with a large V d (29−42 L). While MDRD in patient 1 was low (0.3−0.4 mL s -1 1.7 m -2 ), that of patient 2 was increasing (> 3.1 mL s -1 1.7 m -2 ), which was associated with augmented CL R . In patient 2, the fT reached only 62, 52, and 44% on days 4, 6, and 8, respectively. In patient 1, the %fT was much higher, attaining values four to fivefold greater than that targeted. Conclusions: Critically ill patients are at risk of drug under-or overdosing without dose up-titration with regard to covariate effects and individual drug pharmacokinetics.

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“…10 Cefazolin sodium has some analytical methods described in official compendia such as British, 11 European, 12 Japanese, 13 Portuguese 14 and US 15 pharmacopeias. In the literature, several methods have been described for the qualitative 16 and quantitative analysis of cefazolin sodium, included spectrophotometry, [17][18][19][20][21][22][23][24][25][26][27][28][29] high-performance liquid chromatography [30][31][32][33][34][35][36][37][38][39][40][41][42][43][44][45][46][47] and voltammetry. 48 However, most of them were time-consuming and dedicated to sophisticated and expensive analytical instruments.…”

Section: Introductionmentioning

confidence: 99%

New Environmentally Friendly Method for Quantification of Cefazolin Sodium

Rechelo¹,

Fernandes²,

Kogawa³

et al. 2017

ECB

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Cefazolin sodium, a β-lactam antimicrobial agent belonging to the first generation cephalosporins, has a broad spectrum of action, acting against gram positive and gram negative bacteria. Stands out over other cephalosporins for its ability to also act against some species of Enterobacter, and have a long half-life, thus reducing the frequency of administrations. A simple, fast and reproducible method by visible spectrophotometry was developed and validated for quantification of cefazolin sodium in the lyophilized powder. This technique is widely used in the pharmaceutical industry due to its ease of execution, low cost, safety and high precision and accuracy. It has been employed in the quality control routine of numerous pharmaceuticals in order to identify them and quantify their active principles. The method was capable of detecting and quantifying the cefazolin sodium obtaining satisfactory results regarding selectivity, precision, accuracy and robustness, on linear range of 32.0 to 92.0 µg mL -1 , showing the correlation coefficient of 0.9993 when analyzed at 767 nm. Due to the environmental impacts caused by global economic development, green chemistry has come up with a proposal to minimize and/or eliminate the use of harmful solvents, which generate large amounts of toxic waste to the environment and the health of operators, as well as reducing expenses with costly processes. The proposed method does not use toxic solvent, proving to be effective, low cost, easy to apply and safe for the analyst and environment. *Corresponding AuthorsFax: +55 16 3301 6967 E-Mail: ac_kogawa@yahoo.com.br [a]

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Simultaneous determination of eight β-lactam antibiotics in human serum by liquid chromatography–tandem mass spectrometry

Cited by 111 publications

References 32 publications

Simultaneous determination of seven β-lactam antibiotics in human plasma for therapeutic drug monitoring and pharmacokinetic studies

Simultaneous determination of seven β-lactam antibiotics in human plasma for therapeutic drug monitoring and pharmacokinetic studies

pilot study on pharmacokinetic/pharmacodynamic target attainment in critically ill patients receiving piperacillin/tazobactam

New Environmentally Friendly Method for Quantification of Cefazolin Sodium

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