Liquid–liquid–liquid microextraction followed by HPLC with UV detection for quantitation of ephedrine in urine

Bagheri, Habib; Khalilian, Faezeh; Ahangar, Laleh Enayati

doi:10.1002/jssc.200800193

Cited by 14 publications

(7 citation statements)

References 40 publications

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“…pH of the sample solution plays an important role in liquid–liquid extraction since extraction efficiency is greatly affected by the charge on the analytes. For basic drugs such as Eph, Nor, and Pse, aqueous sample solutions were commonly strongly alkalized to keep the analytes in their neutral form and consequently reduce their solubility in the urine matrix . The influence of sample pH on extraction efficiency was studied over the range 7.0–13.0.…”

Section: Resultsmentioning

confidence: 99%

Ultrasound‐assisted emulsification microextraction for the determination of ephedrines in human urine by capillary electrophoresis with direct injection. Comparison with dispersive liquid–liquid microextraction

Alshana¹,

Göǧer²,

Ertaş

2012

J of Separation Science

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Ultrasound-assisted emulsification microextraction and dispersive liquid-liquid microextraction were compared for extraction of ephedrine, norephedrine, and pseudoephedrine from human urine samples prior to their determination by capillary electrophoresis. Formation of a microemulsion of the organic extract with an aqueous solution (at pH 3.2) containing 10% methanol facilitated the direct injection of the final extract into the capillary. Influential parameters affecting extraction efficiency were systematically studied and optimized. In order to enhance the sensitivity further, field-amplified sample injection was applied. Under optimum extraction and stacking conditions, enrichment factors of up to 140 and 1750 as compared to conventional capillary zone electrophoresis were obtained resulting in limits of detection of 12-33 μg/L and 1.0-2.8 μg/L with dispersive liquid-liquid microextraction and ultrasound-assisted emulsification microextraction when combined with field-amplified sample injection. Calibration graphs showed good linearity for urine samples by both methods with coefficients of determination higher than 0.9973 and percent relative standard deviations of the analyses in the range of 3.4-8.2% for (n = 5). The results showed that the use of ultrasound to assist microextraction provided higher extraction efficiencies than disperser solvents, regarding the hydrophilic nature of the investigated analytes.

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Section: Resultsmentioning

confidence: 99%

Ultrasound‐assisted emulsification microextraction for the determination of ephedrines in human urine by capillary electrophoresis with direct injection. Comparison with dispersive liquid–liquid microextraction

Alshana¹,

Göǧer²,

Ertaş

2012

J of Separation Science

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“…In this case, ephedrine in herbal medicines needs to be detected and any excess should be removed. Common detection methods include high‐performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE), and some related methods have already been applied to detect ephedrine in internet‐available drugs, medicines or urine samples . In order to remove ephedrine, solid‐phase extraction (SPE) is one of the most efficient methods .…”

Section: Introductionmentioning

confidence: 99%

Multi‐phase extraction of ephedrine from Pinellia ternata and herbal medicine using molecular imprinted polymer coated ionic liquid‐based silica

Fang

Xie

Lin

et al. 2019

Phytochemical Analysis

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Introduction Ephedrine is a typical compound found in lots of plant species that is used in several medicines for the treatment of asthma and bronchitis. However, excess amounts are harmful to humans, so it needs to be removed. Objective This study developed a multi‐phase extraction (MPE) method with a molecular imprinted polymer (MIP) coated ionic liquid (IL)‐based silica (SiO2@IL@MIP) to simultaneously extract and separate ephedrine from Pinellia ternata, 10 medicines, and urine samples. Methods IL was immobilized on silica. Subsequently, the IL was combined with the functional monomer, followed by the addition of the crosslinker and template. The resulting sorbent was applied to the MPE, and the extraction, washing and elution solvents were evaluated. Results Fourier‐transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the synthesis of SiO2@IL@MIP. A maximum adsorption amount of 5.76 mg/g was obtained at 30°C at a neutral pH. In MPE, 10.00 mL of methanol could extract all the ephedrine from Pinellia ternata. The interference was removed by washing with 4.00 mL of water, ethanol, and acetonitrile. Finally, 8.00 mL of methanol/acetic acid (99:1, v/v) was applied as the elution solvent. The following were extracted: 5.50 μg/g of ephedrine from Pinellia ternata, 0.00–46.50 μg/g from the 10 herbal medicines, and 68.70–102.80 μg/mL in the urine samples. Conclusion The proposed method was applied successfully to the simultaneously extraction and separation of ephedrine from plants and medicines. These results are expected to provide important data for the development of new methods for the separation and purification of bioactive compounds.

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“…In recent years, miniaturization is one noticeable trend, such as solid phase microextraction (SPME), 26,27 supported liquid membrane extraction (SLME) 28,29 and liquid phase microextraction (LPME). 30,31 However, current trends in sample preparation are focused on the use of low solvent consumption miniaturized methods, among which LPME has experienced great success in the last decades. In fact, LPME has found a signicant place in the extraction and concentration of target compounds from certain complex extracts.…”

Section: Introductionmentioning

confidence: 99%

Determination of 2-methoxyestradiol from endometrial cancer patients' urine by LC-MS/MS with hollow fiber liquid-phase microextraction

Liu

et al. 2013

Anal. Methods

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2-Methoxyestradiol (2-MeOE 2 ) is a potent antiangiogenic and antitumor agent in preclinical models due to its antiproliferative and apoptotic actions. In endometrial cancer patients' urine, the content of 2-MeOE 2 may be less than that in urine samples of healthy people. The sensitivity can be elevated to a high level by using hollow fiber liquid-phase microextraction (HF-LPME) as an enriched pretreatment method with LC-MS/MS as a detection means. In the experimental section, the urine sample was firstly handled with sodium hydroxide for hydrolysis and then extracted with HF-LPME. After that the extracts were derivatised and finally detected with LC-MS/MS. For HF-LPME, we obtained an enrichment factor of 180 along with a good sample clean-up. The calibration curve was linear with a linear regression correlation coefficient typically greater than 0.996. The limit of detection (LOD) for 2-MeOE 2 was 0.14 pg mL À1 with good repeatability and reproducibility. The proposed method was applied for the analysis of human urine samples from endometrial cancer patients and healthy people.

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Liquid–liquid–liquid microextraction followed by HPLC with UV detection for quantitation of ephedrine in urine

Cited by 14 publications

References 40 publications

Ultrasound‐assisted emulsification microextraction for the determination of ephedrines in human urine by capillary electrophoresis with direct injection. Comparison with dispersive liquid–liquid microextraction

Ultrasound‐assisted emulsification microextraction for the determination of ephedrines in human urine by capillary electrophoresis with direct injection. Comparison with dispersive liquid–liquid microextraction

Multi‐phase extraction of ephedrine from Pinellia ternata and herbal medicine using molecular imprinted polymer coated ionic liquid‐based silica

Determination of 2-methoxyestradiol from endometrial cancer patients' urine by LC-MS/MS with hollow fiber liquid-phase microextraction

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