In-process control of midazolam synthesis by HPLC

Laviana, L.; Llorente, Isabel Santiago; Bayod, Miguel; Blanco, Domingo

doi:10.1016/s0731-7085(03)00057-8

Cited by 10 publications

(5 citation statements)

References 22 publications

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“…There are also a few papers referring to the determination of the impurities in the active pharmaceutical ingredients (API) of bosentan monohydrate and compounds generated during the degradation study [1, 19, 20]. Some papers deal with the analysis of the in-process control (IPC) of the API [21, 22]; however, there is no uniform requirement to follow the guidelines for the IPC methods.…”

Section: Introductionmentioning

confidence: 99%

“…There are only a few publications describing spectrophotometric methods for the estimation of bosentan monohydrate in pharmaceutical dosage forms [ 15 – 17 ]. The majority of analytical papers concern HPLC with UV and MS detection as the techniques used for the separation and determination of bosentan, its metabolites and degradation products [ 8 – 14 , 18 – 22 ]. The analytical procedure was published in the authorized USP Pending Monograph and in the United States Pharmacopeia Convention.…”

Section: Introductionmentioning

confidence: 99%

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Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

et al. 2016

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Bosentan monohydrate (4-tert-butyl-N-[6-(2-hydroxyethoxy)-5-(2-methoxyphenoxy)-2-(pyrimidin-2-yl) pyrimidin-4-yl]benzene-1-sulfonamide monohydrate) is a dual endothelin receptor antagonist (ERA) applied in the treatment of pulmonary arterial hypertension. To achieve effective process control of the bosentan monohydrate synthesis, it was necessary to develop a selective and not highly time-consuming method for ultra-high performance liquid chromatography (UHPLC). The method is characterized by adequate sensitivity, reproducibility and selectivity for the determination of bosentan monohydrate and related compounds from all synthetic stages. The UHPLC separation was carried out by reversed phase chromatography on the Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 µm) with a mobile phase composed of solvent A (0.1 %, v/v, acetic acid in water) and solvent B (methanol), in the gradient mode at the flow rate of 0.4 mL min−1. Limits of detection and quantification for the compounds were ≤0.1 µg mL−1 and 0.3 µg mL−1, respectively. The linearity for all related compounds was investigated as in the range for the active pharmaceutical ingredient (API) and as in the range for the in-process control. The developed method was validated according to the current guidelines, proving the suitability of the method for its intended purpose.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

et al. 2016

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“…[7] After an enquiry to the producer of the midazolam drug commonly used in Germany (Dormicum W ), the use of desalkylflurazepam as a starting substance was confirmed. In many pharmaceutical laboratories, HPLC-PDA is still a common method applied for the in-process control of synthesis [7] because it complies with the pharmaceutical requirements concerning purity.…”

Section: Discussionmentioning

confidence: 99%

Desalkylflurazepam found in patients’ samples after high‐dose midazolam treatment

Vogt

Kempf

Buttler

et al. 2013

Drug Testing and Analysis

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“…These include gas chromatography, 15 spectrophotometry, 16 and liquid chromatography 17 coupled with mass spectrometry, which has been applied for the determination of KET and its metabolites in biological samples such as urine. 18 However, these methods require a large number of samples and reagents, access to centralized laboratories, a longer time of training for the analyst, and are costly because of their sophisticated instrumentation. 19,20 As opposed to these requirement, the modern trend for miniaturized, low power, and low-cost portable devices has led to the development of electrochemical sensors for screening of drugs of abuse.…”

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confidence: 99%

Textile-based wearable device for detection of date rape drugs in drinks

Stojanović,

Milić,

Endro

et al. 2023

Textile Research Journal

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In this article, a sensing element for detection of date rape drugs in drinks is presented. The element consists of a three-dimensional printed holder, in which two embroidered electrodes have been fixed, forming a capacitive structure. As the dielectric properties of the liquid between these electrodes’ changes, the capacitance and consequently the impedance are changed. For experimental purposes, diazepam, a model rape drug, sucrose, and sodium chloride, which are used as control ingredients, were dissolved in a 40% V/V alcoholic beverage, serving as solutions for testing and comparison. The selectivity, repeatability, and sensitivity of the proposed sensor were tested. The sensitivity of detection of 1 mg/ml of diazepam in drinks was 0.92628 Ωl/mg, sucrose was 0.94774 Ωl/mg and sodium chloride was 2.46867 Ωl/mg, at 1 MHz. Moreover, with the use of the Cole impedance model, the selectivity of the sensor in the detection of diazepam, through the Nyquist plot and parameter estimation, has been achieved. Sensor repeatability was calculated through the relative standard deviation with the result for 1 mg/ml of diazepam dissolved in alcohol on 1 MHz being 2.48, in terms of impedance modulus. The presented sensor platform can successfully detect drugs in drinks and can protect from many cases of such assaults in a real world.

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In-process control of midazolam synthesis by HPLC

Cited by 10 publications

References 22 publications

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

Desalkylflurazepam found in patients’ samples after high‐dose midazolam treatment

Textile-based wearable device for detection of date rape drugs in drinks

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