Solid phase micro‐extraction coupled with ion mobility spectrometry for the analysis of ephedrine in urine

Lokhnauth, John K.; Snow, Nicholas H.

doi:10.1002/jssc.200401924

Cited by 51 publications

(32 citation statements)

References 26 publications

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“…Several methods of such couplings were already proposed. [30][31][32][33][34][35][36] Current attempts are being made to select the platforms and determine the most efficient method for on-site use. As well, investigations are being conducted to determine the best solution for different groups of compounds and specific biomarkers characterized by different properties.…”

Section: Noninvasive Monitoring Metabolic Changes Through Perfusate Smentioning

confidence: 99%

Low invasive in vivo tissue sampling for monitoring biomarkers and drugs during surgery

Bojko

Goryński

Gómez‐Ríos

et al. 2014

Laboratory Investigation

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The techniques currently used for drug, metabolite, and biomarker determination are based on sample collection, and therefore they are not suitable for repeated analysis because of the high invasiveness. Here, we present a novel method of biochemical analysis directly in organ during operation without need of a separate sample collection step: solid-phase microextraction (SPME). The approach is based on flexible microprobe coated with biocompatible extraction phase that is inserted to the tissue with no damage or disturbance of the organ. The method was evaluated during lung and liver transplantations using normothermic ex vivo liver perfusion (NEVLP) and ex vivo lung perfusion (EVLP). The study demonstrated feasibility of the method to extract wide range of endogenous compounds and drugs. Statistical analysis allowed observing metabolic changes of lung during cold ischemic time, perfusion, and reperfusion. It was also demonstrated that the level of drugs and their metabolites can be monitored over time. Based on the methylprednisolone as a selected example, the impairment of enzymatic properties of liver was detected in the injured organs but not in healthy control. This finding was supported by changes in pathways of endogenous metabolites. The SPME probe was also used for analysis of perfusion fluid using stopcock connection. The evaluation of biochemical profile of perfusates demonstrated potential of the approach for monitoring organ function during ex vivo perfusion. The simplicity of the device makes it convenient to use by medical personnel. With the microprobe, different areas of the organ or various organs can be sampled simultaneously. The technology allows assessment of organ function by biochemical profiling, determination of potential biomarkers, and drug monitoring. The use of this method for preintervention analysis could enhance the decision-making process for the best possible personalized approach, whereas post-transplantation monitoring would be used for graft assessments and fast response in case of organ failure.

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Section: Noninvasive Monitoring Metabolic Changes Through Perfusate Smentioning

confidence: 99%

Low invasive in vivo tissue sampling for monitoring biomarkers and drugs during surgery

Bojko

Goryński

Gómez‐Ríos

et al. 2014

Laboratory Investigation

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“…Thus, a quantification method for this drug in biological fluids (e.g., urine, serum, and saliva) is of great interest for doping control purpose. Ephedrine becomes widely distributed by the circulatory system, and is eliminated by first order kinetics via the urinary system, with the analysis of the urine being the primary tool for quantitation of ephedrine in doping cases [14]. The IOC has set a permitted level of 10 lg/mL.…”

Section: Introductionmentioning

confidence: 99%

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

Bagheri¹,

Khalilian²,

Ahangar³

2008

J of Separation Science

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Liquid-liquid-liquid microextraction (LLLME) in combination with HPLC and UV detection has been used as a sensitive method for the determination of ephedrine in urine samples. Extraction process was performed in a homemade total glass vial without using a Teflon ring, usually employed. Ephedrine was first extracted from 3.5 mL of urine sample (pH 12) into a microfilm of toluene/benzene (50:50). The analyte was subsequently back extracted into an acidic microdrop solution (pH 2) suspended in the organic phase. The extract was then injected into the HPLC system directly. An enrichment factor of 137 along with a good sample clean-up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 0.01-50 mg/L with regression coefficient corresponding to 0.998. The LODs and LOQs, based on a S/N of 3 and 10, were 5 and 10 microg/L, respectively. The method was eventually applied for the determination of ephedrine in urine sample after oral administration of 5 mg single dose of drug.

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“…Many methods have been developed to quantify ephedrines in urine, including the gas chromatography nitrogen phosphorous detector (GC-NPD), 8 GC mass spectrometry (GC-MS), 9 ion mobility MS (IM-MS) 10 and liquid chromatography MS in tandem (LC-MS/MS). 11 Among them, LC-MS/MS is the most frequently used method, enabling the direct injection of dilute urine into the chromatographic system.…”

Section: Introductionmentioning

confidence: 99%

“…[14][15][16] All other methods described, including the GC-based ones, require sample pretreatment such as liquid-liquid extraction, solid-phase extraction and/or filtration, which is time-consuming and reduces the sample throughput . [8][9][10]17 The application of GC analysis to quantify ephedrines was first developed in 1977 by Lin et al 18 They used a specific electron-capture assay after a liquid-liquid extraction with benzene and trifluoroacetic acid (TFA) derivatives to detect pseudoephedrine and norpseudoephedrine. 18 Subsequently, the GC method to determine ephedrine was modified to reduce the toxicity of sample preparation and improve the sensitivity using toluene as the extraction solvent and trifluoroacetic anhydride (TFAA).…”

Section: Introductionmentioning

confidence: 99%

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

Carneiro¹,

Silva²,

Cavalcante³

et al. 2018

J. Braz. Chem. Soc.

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Ephedrines are widely used in therapy. Because of their stimulant properties, these substances are relevant in different forensic fields. At present, the state of the art for ephedrines quantification relay based on a liquid chromatography mass spectrometry, mainly because of the dilute-andshoot approach. Notwithstanding, several gas chromatography based methods have already been described, all of them include cleanup steps, with the potential disadvantage of incurring errors and increasing the workload. In this paper, a straightforward method for ephedrine quantification based on gas chromatographic mass spectrometry, without cleanup and based on Doehlert matrix optimization is presented. Only 10 µL of a urine sample is necessary and for N-methyl-N-(trimethylsilyl)trifluoroacetamide/N-methyl-bis-trifluoracetamide derivatives, the intermediate precision was 2.77% for ephedrine, 9.20% for cathine, 8.29% for norephedrine and 4.27% for pseudoephedrine. The limit of detection was 20 ng mL -1 for ephedrine, 30 ng mL -1 for cathine and 40 ng mL -1 for norephedrine and pseudoephedrine.

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Solid phase micro‐extraction coupled with ion mobility spectrometry for the analysis of ephedrine in urine

Cited by 51 publications

References 26 publications

Low invasive in vivo tissue sampling for monitoring biomarkers and drugs during surgery

Low invasive in vivo tissue sampling for monitoring biomarkers and drugs during surgery

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

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

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