An UHPLC–MS/MS Method for The Simultaneous Determination of Ampicillin and Sulbactam in Human Plasma and Urine

Parker, Suzanne L.; Adnan, Syamhanin; Meija, Jenny L Ordóñez; Paterson, David L.; Lipman, Jeffrey; Roberts, Jason A.; Wallis, Steven C.

doi:10.4155/bio.15.143

Cited by 10 publications

(8 citation statements)

References 22 publications

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“…37 Therefore, it is of great importance to ensure the level of ampicillin in biological fluids is above the MIC for extended periods of time without overdosing to mitigate the adverse effects. 38 Urine ampicillin has been detected using HPLC, but all those methods require extensive sample pretreatment such as extraction, purification, and preconcentration before analysis. 38−40 For analysis using the 3D printed microdevice, a small aliquot of fluorescamine was added to urine samples from a healthy volunteer, spiked and nonspiked with ampicillin.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Figure 5b shows a linear increase in peak height with concentration and the range 0−100 ppm examined covers the urine level measured using other methods. 38,39,41 The relative standard deviation (RSD) for the analysis of a urine sample spiked with 25 ppm ampicillin was 21% (n = 3 devices). In this 3D printed device, the analytical workflow for the quantitation of ampicillin was conducted in just over 5 min, using a small sample volume (10 μL) and minimal manual handling.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Some side effects of ampicillin such as diarrhea, rash, nausea, etc., have been reported when the concentration is too high . Therefore, it is of great importance to ensure the level of ampicillin in biological fluids is above the MIC for extended periods of time without overdosing to mitigate the adverse effects . Urine ampicillin has been detected using HPLC, but all those methods require extensive sample pretreatment such as extraction, purification, and preconcentration before analysis. − …”

Section: Resultsmentioning

confidence: 99%

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Multimaterial 3D Printed Fluidic Device for Measuring Pharmaceuticals in Biological Fluids

Macdonald

Guijt

et al. 2018

Anal. Chem.

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Multimaterial 3D printing provides a unique capability for the creation of highly complex integrated devices where complementary functionality is realized using differences in material properties. Using a single and automated print process, microfluidic devices were fabricated containing (i) an optically transparent structure for fluorescence detection, (ii) electrodes for electrokinetic transport, (iii) a primary membrane to remove particulates and macromolecules including proteins, and (iv) a secondary membrane to concentrate small molecule targets. The device was used for the simultaneous extraction and concentration of small molecule pharmaceuticals from urine, which was followed by an on-chip electrophoretic separation of the concentrated targets for quantitative analysis. Owing to the high level of functional integration inside the device, manual handling was minimal and restricted to the introduction of the sample and buffer solutions. The 3D printed sample-in/answerout device allowed the direct quantification of ampicillina small molecule pharmaceuticalin untreated urine within 3 min, down to 2 ppm. These results demonstrate the potential of 3D printing for on-demand fabrication of disposable, functionally integrated devices for low-cost point-of-collection (POC) diagnostics.P oint-of-collection (POC) testing requires the ability to detect and quantify analytical target(s) directly from a complex sample without user intervention. The field is dominated by tests that exploit the exquisite selectivity of antibodies and/or enzymes; however for small molecule targets, such as many biomarkers, pharmaceuticals, and their metabolites, cross-selectivity may lead to inaccurate results. 1 Larger laboratory-housed instrumentation, such as chromatographs and mass spectrometers, are currently used to quantify these small molecules using a time-and cost-intensive process. The next evolution of POC devices is the miniaturization and translation of this instrumentation into small portable devices to provide quantitative POC small molecule analysis capability. This concept, first discussed in the early 1990s, 2 has proven difficult to realize because of the technical difficulty in fabricating devices capable of accommodating complex and disparate chemical processes in a simple, affordable, and automated manner. 3,4 For example, a typical workflow for the analysis of pharmaceuticals from blood/serum/plasma in a laboratory setting requires extraction of the targets from the sample, frequently involving a volume reduction step, followed by separation on a liquid chromatograph with mass spectrometry detection. 5 An integrated device for POC testing must contain all of the structures, materials, and reagents for a similar but automated workflow.Currently the most cost-effective approach to manufacture microfluidic devices is using mass-replication techniques, such as injection molding or hot embossing, as these allow thousands of polymeric devices to be made a day. However, the incorporation of different materials and reagen...

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Section: ■ Results and Discussionmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

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Multimaterial 3D Printed Fluidic Device for Measuring Pharmaceuticals in Biological Fluids

Macdonald

Guijt

et al. 2018

Anal. Chem.

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“…The extensive literature survey revealed that several analytical techniques, likely as high-performance liquid chromatography (HPLC) [2,3], capillary electrophoresis (CE) [4,5], Fouriertransform infrared spectroscopy (FTIR) [6] were available for the determination in bulk and pharmaceutical formulations. It can be quantified with liquid chromatography-mass spectrophotometry (LCMS) [7] and ultra-performance liquid chromatography-mass spectrophotometry (UPLC-MS) [8] in biological fluids. Most of the techniques are involved with the complicated procedure, extraction with toxic solvents, and expensive instrumentation and pretreatment of the sample before analysis.…”

Section: Introductionmentioning

confidence: 99%

Optimized and Validated Spectrophotometric Method for the Determination of Ampicillin in Pharmaceutical Formulations

Haque

2021

Int J Pharm Pharm Sci

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Objective: A simple, precise, and accurate spectrophotometric method has been developed to determine Ampicillin in pharmaceutical formulations. Methods: The proposed method, based on the carboxylic acid group reaction, present in Ampicillin with a mixture of KIO3 and KI, form a yellow-colored product in an aqueous medium. The response was allowed to proceed at 25±1 °C, and absorbance measured after 5 min against a reagent blank prepared simultaneously using a UV-Vis spectrophotometer. The parameters verified were specificity, linearity, linearity range, accuracy, precision, detection limit, quantitation limit, robustness, and ruggedness. Results: The yellow-colored product was measured at 352 nm against the reagent blank using UV–Vis spectrophotometer. The linear dynamic range of concentration was 0.25–2.5 µg/ml with a correlation coefficient of 0.9999. The LOD, LOQ values to be 0.086 and 0.261 µg/ml, respectively, for the proposed method. The percentage of recoveries was 98.27–100.89% with an acceptable relative standard deviation (±2%). The robustness and ruggedness values were excellent. Conclusion: The ICH guidelines for pharmaceuticals and human use were followed and applied to validate the proposed method. The method was compared with available literature and found similar results that confirmed the reliability and effective way for Ampicillin's determination.

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“…Although several studies reported measuring AMP or SUL individually, only a few studies have analyzed both AMP and SUL. UHPLC-MS/MS and HPLC-UV methods have been employed for the quantification of AMP/SUL in bovine milk (12) and in pharmaceutical preparations (13). On the other hand, LC-MS and LC-MS/MS methods have been recently used for the analysis of plasma PARA as well as urine metabolites, either individually or with other concomitantly given drugs (14)(15)(16).…”

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confidence: 99%

A green approach to the analysis of co-administered ampicillin/sulbactam and paracetamol in human urine

et al. 2021

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The novelty of this work is the simultaneous analysis of sulbactam (SUL), ampicillin (AMP), and paracetamol (PARA) in human urine samples, using the environmentally benign RP-HPLC method. A C18 column was used in chromatographic separation using potassium dihydrogen phosphate (10 mmol L–1, pH 5)/ethanol (90 %, V/V) as the mobile phase; flow rate was 1.00 mL min–1. UV detection at 220 nm was used for quantification. The proposed method showed good linearity in the concentration ranges of 2.20–250.00 μg mL–1 for SUL, 2.50–250.00 μg mL–1 for PARA, and 14.50–250.00 μg mL–1 for AMP. Direct injection of urine samples with no prior extraction was performed. This method was found successful in moving towards greener studies of drugs’ urinary excretion, by decreasing hazardous solvent consumption and waste. Moreover, the method was applied to investigate the urinary excretion of the drugs and possible interaction between ampicillin and paracetamol.

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An UHPLC–MS/MS Method for The Simultaneous Determination of Ampicillin and Sulbactam in Human Plasma and Urine

Abstract: An UHPLC-MS/MS method to simultaneously measure co-formulated ampicillin and sulbactam in plasma and urine, for use in a patient PK study, has been developed and validated.

Cited by 10 publications

References 22 publications

Multimaterial 3D Printed Fluidic Device for Measuring Pharmaceuticals in Biological Fluids

Multimaterial 3D Printed Fluidic Device for Measuring Pharmaceuticals in Biological Fluids

Optimized and Validated Spectrophotometric Method for the Determination of Ampicillin in Pharmaceutical Formulations

A green approach to the analysis of co-administered ampicillin/sulbactam and paracetamol in human urine

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