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Development of a Efficient and Sensitive Dispersive Liquid-Liquid Microextraction Technique for Extraction and Preconcentration of 10 ?2-Agonists in Animal Urine.

ABSTRACT: Dispersive liquid-liquid microextraction (DLLME) coupled with ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) was developed for the extraction and determination of 10 ?2-agonists in animal urine. Some experimental parameters, such as the type and volume of the extraction solvent, the concentration of the dispersant, the salt concentration, the pH value of the sample solution, the extraction time and the speed of centrifugation, were investigated and optimized. Under the optimized conditions, a good enrichment factors (4.8 to 32.3) were obtained for the extraction. The enrichment factor show that the concentration rate of DLLME is significantly higher than other pretreatment methods, and the detection sensitivity has been greatly improved. The calibration curves were linear, the correlation coefficient ranged from 0.9928 to 0.9999 for the concentration range of 0.05 to 50 ng mL(-1) and 0.1 to 50 ng mL(-1), and the relative standard deviations (RSDs, n = 15, intra and inter-day precision) at a concentration of 5 ng mL(-1) were in the range of 1.8 to 14.6%. The limits of detection (LODs) for the 10 ?2-agonists, based on a signal-to-noise ratio (S/N) of 3, were in the range of 0.01 to 0.03 ng mL(-1). The proposed method was used to identify ?2-agonists in three types of animal urine (swine, cattle, sheep), and the relative recoveries from each matrix were in the range of 89.2 to 106.8%, 90.0 to 109.8% and 89.2 to 107.2%, respectively.

SUBMITTER: Li Y

PROVIDER: S-EPMC4562641 | biostudies-literature | 2015

REPOSITORIES: biostudies-literature

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Publications

Development of a Efficient and Sensitive Dispersive Liquid-Liquid Microextraction Technique for Extraction and Preconcentration of 10 β2-Agonists in Animal Urine.

Li Yang Y Zhang Wei W Wang Rui-Guo RG Wang Pei-Long PL Su Xiao-Ou XO

PloS one 20150908 9

Dispersive liquid-liquid microextraction (DLLME) coupled with ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) was developed for the extraction and determination of 10 β2-agonists in animal urine. Some experimental parameters, such as the type and volume of the extraction solvent, the concentration of the dispersant, the salt concentration, the pH value of the sample solution, the extraction time and the speed of centrifugation, were investigated and optimized. ...[more]

PMID: 26348922

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Project description:In recent years, therapeutic drug monitoring (TDM) has been applied in docetaxel (DOC)-based anticancer therapy to precisely control various pharmacokinetic parameters, including the concentration of DOC in biofluids (e.g., plasma or urine), its clearance, and its area under the curve (AUC). The ability to determine these values and to monitor DOC levels in biological samples depends on the availability of precise and accurate analytical methods that both enable fast and sensitive analysis and can be implemented in routine clinical practice. This paper presents a new method for isolating DOC from plasma and urine samples based on the coupling of microextraction and advanced liquid chromatography with tandem mass spectrometry (LC-MS/MS). In the proposed method, biological samples are prepared via ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) using ethanol (EtOH) and chloroform (Chl) as the desorption and extraction solvents, respectively. The proposed protocol was fully validated according to the Food and Drug Administration (FDA) and the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) requirements. The developed method was then applied to monitor the DOC profile in plasma and urine samples collected from a pediatric patient suffering from cardiac angiosarcoma (AS) with metastasis to lungs and mediastinal lymph nodes, who was receiving treatment with DOC at a dose of 30 mg/m2 body surface area. Due to the rarity of this disease, TDM was carried out to determine the exact levels of DOC at particular time points to ascertain which levels were conducive to maximizing the treatment's effectiveness while minimizing the drug's toxicity. To this end, the concentration-time profiles of DOC in the plasma and urine samples were determined, and the levels of DOC at specific time intervals up to 3 days after administration were measured. The results showed that DOC was present at higher concentrations in the plasma than in the urine samples, which is due to the fact that this drug is primarily metabolized in the liver and then eliminated with the bile. The obtained data provided information about the pharmacokinetic profile of DOC in pediatric patients with cardiac AS, which enabled the dose to be adjusted to achieve the optimal therapeutic regimen. The findings of this work demonstrate that the optimized method can be applied for the routine monitoring of DOC levels in plasma and urine samples as a part of pharmacotherapy in oncological patients.

Dataset Information

Development of a Efficient and Sensitive Dispersive Liquid-Liquid Microextraction Technique for Extraction and Preconcentration of 10 ?2-Agonists in Animal Urine.

Publications

Development of a Efficient and Sensitive Dispersive Liquid-Liquid Microextraction Technique for Extraction and Preconcentration of 10 β2-Agonists in Animal Urine.

Similar Datasets

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