A manual shaking-enhanced, ultrasound-assisted dispersive liquid–liquid microextraction for the determination of betamethasone and dexamethasone: optimization using Response surface methodology

Shamsipur, Mojtaba; Jouybari, Touraj Ahmadi; Barati, Ali; Mahmoudi, Majid; Amin, Niloufar; Pashabadi, Afshin

doi:10.1039/c4ay00373j

Cited by 6 publications

(4 citation statements)

References 42 publications

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“…Compared with previously reported extractants such as methyl tert-butyl ether (MTBE), 24 diethyl ether-hexamethylene, 4 acetone-chloroform (5 : 1, v/v), 9 ether-cyclohexane (4 : 1, v/v) 6 and methylene chloride, 8 ether/n-hexane (4 : 1, v/v) was chosen as an ideal solvent to extract the BDP, BOH, B17P and B21P with high extraction efficiency and minimal matrix effects. But a non-negligible drawback of LLE was that hydrophilic compounds could not be extracted by a water-immiscible solvent.…”

Section: Resultsmentioning

confidence: 97%

“…In the past decades, most of the validated HPLC-MS/MS were used for the quantification of BDP, BOH and B17P in both drug formulations and biological samples, 4-6, 8, 9, 28 but few methods were developed for the determination of BSP and B21P in human plasma. Although BSP was not detected in the collected human plasmas from the healthy subjects due to its rapid degradation in human body, the validated method might be useful for the determination of the sustained-release preparations containing BSP developed in the future.…”

Section: Resultsmentioning

confidence: 99%

“…As synthesized glucocorticoids, their adverse effects are inevitable ranging from skin fragility to full-blown iatrogenic Cushing syndrome such as obesity, hypertension, osteoporosis and other diseases. 8,9 Prolonged use of BSP and BDP may lead to suppression of the hypothalamic-pituitary-adrenal axis due to the impact on endogenous cortisol concentration as well as a circadian pattern. 8,10 Moreover, as a kind of antenatal steroid therapy to prevent respiratory distress syndrome in premature neonates, it had been reported that maternal betamethasone administration could cause the risk of fetal growth restriction and preterm birth.…”

Section: Introductionmentioning

confidence: 99%

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Quantitative determination of betamethasone sodium phosphate and betamethasone dipropionate in human plasma by UPLC-MS/MS and a bioequivalence study

et al. 2016

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The compound medicine of betamethasone sodium phosphate (BSP) and betamethasone dipropionate (BDP) is widely used for diverse glucocorticoid-sensitive acute and chronic diseases such as asthma, rheumatoid arthritis and systemic lupus erythematosus. It will be useful and beneficial to validate sensitive method for the determination of BSP, BDP and their metabolites for their pharmacokinetic study. Hereby, an ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been validated for the determination of BSP, BDP and their metabolites betamethasone (BOH), betamethasone 17-monodipropionate (B17P) and betamethasone 21-monodipropionate (B21P) in human plasma. Liquid-liquid extraction with ether and n-hexane (v/v, 4:1) was used for sample preparation of BDP, BOH, B17P and B21P with beclomethasone dipropionate as internal standard (IS), while solid phase extraction was adopted for sample preparation of BSP using prednisolone as IS. The chromatographic separation was performed on a Hypurity C18 column (150 mm×2.1 mm, 5 μm) for BOH, BDP, B21P and B17P, and a Luna C18 (2) column (150 mm×2.0 mm, 5 μm) for BSP. Electrospray ionization interfaced with positive multiple reaction monitoring (MRM) scan mode was used for mass spectrometric detection. The standard calibration curves were linear within the range of 2.525 × 10−9−403.9 × 10−9 mol·dm−3 for BSP, 0.125 × 10−9−55.81 × 10−9 mol·dm−3 for BDP, 0.278 × 10−9−74.95 × 10−9 mol·dm−3 for BOH, 0.098 × 10−9−4.688 × 10−9 mol·dm−3 for B17P and 0.226 × 10−9−5.411 × 10−9 mol·dm−3 for B21P, respectively. The validated method was successfully applied to a bioequivalence study in 23 healthy subjects after they were injected with this compound medicine BSP and BDP.

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Section: Resultsmentioning

confidence: 97%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Quantitative determination of betamethasone sodium phosphate and betamethasone dipropionate in human plasma by UPLC-MS/MS and a bioequivalence study

et al. 2016

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“…Later, other types of liquid-liquid microextraction (LLME) techniques, such as headspace liquid-phase microextraction (HS-LPME), [5][6][7] hollow ber liquid-liquid microextraction (HF-LLME), 8-10 vortex-assisted liquid-liquid microextraction (VALLME) [11][12][13] and dispersive liquid-liquid microextraction (DLLME), [14][15][16][17] were developed. These methods have many advantages such as a reduction in the required sample and solvent, a high enrichment factor and a clean-up step.…”

Section: Introductionmentioning

confidence: 99%

Development of combined salt- and air-assisted liquid–liquid microextraction as a novel sample preparation technique

Heydari

Zarabi

2014

Anal. Methods

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Vortex-assisted surfactant-enhanced emulsification microextraction combined with LC–MS/MS for the determination of glucocorticoids in water with the aid of experimental design

2017

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An efficient and inexpensive method using vortex-assisted surfactant-enhanced emulsification microextraction (VASEME) based on solidification of floating organic droplet coupled with ultraperformance liquid chromatography-tandem mass spectrometry is proposed for the analysis of glucocorticoids in water samples (river water and hospital wastewater). VASEME was optimized by the experimental validation of Plackett-Burman design and central composite design, which has been co-related to experimental design. Plackett-Burman design showed that factors such as vortex time, surfactant concentration, and pH significantly affect the extraction efficiency of the method. Method validation was characterized by an acceptable calibration range of 1-1000 ng L, and the limit of detection was in the range from 2.20 to 8.12 ng L for glucocorticoids. The proposed method was applied to determine glucocorticoids in river water and hospital wastewater in Lucknow, India. It is reliable and rapid and has potential application for analysis of glucocorticoids in environmental aqueous samples. Graphical Abstract Low density based extraction of gluococorticoids by using design of experiment.

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A manual shaking-enhanced, ultrasound-assisted dispersive liquid–liquid microextraction for the determination of betamethasone and dexamethasone: optimization using Response surface methodology

Cited by 6 publications

References 42 publications

Quantitative determination of betamethasone sodium phosphate and betamethasone dipropionate in human plasma by UPLC-MS/MS and a bioequivalence study

Quantitative determination of betamethasone sodium phosphate and betamethasone dipropionate in human plasma by UPLC-MS/MS and a bioequivalence study

Development of combined salt- and air-assisted liquid–liquid microextraction as a novel sample preparation technique

Vortex-assisted surfactant-enhanced emulsification microextraction combined with LC–MS/MS for the determination of glucocorticoids in water with the aid of experimental design

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