Pharmaceutical Analysis Research Center and Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran; Student Research Committee, Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran.
Tuberculosis and Lung Diseases Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Sep 1;1152:122256. doi: 10.1016/j.jchromb.2020.122256. Epub 2020 Jun 25.
In this work, a microwave-enhanced air-assisted liquid-liquid microextraction method combined with gas chromatography-mass spectrometry has been developed for morphine and oxymorphone assessment in EBC samples. For this purpose, choline chloride-menthol-phenylacetic acid deep eutectic solvent (as an extraction solvent), butyl chloroformate (as a derivatization agent), and picoline (as a catalyst) are used. After performing predetermined extraction cycles in the microextraction method, the obtained cloudy solution is exposed to microwave irradiations to enhance extraction and derivatization efficiencies. The method provided low limits of detection (morphine 2.1 and oxymorphone 1.5 ng mL) and quantification (morphine 7.2 and oxymorphone 5.2 ng mL) in the EBC samples. The method had proper repeatability, accuracy, and stability expressed as relative standard deviations less than 5.1, 9, and 9%, respectively. The developed method was successfully used to determine morphine and oxymorphone concentrations in the EBC samples of addict patients.
本工作建立了一种微波辅助空气辅助液-液微萃取方法，并结合气相色谱-质谱法，用于测定呼出气冷凝物（EBC）样品中的吗啡和羟吗啡。为此，采用了氯化胆碱-薄荷醇-苯乙酸深共晶溶剂（作为萃取溶剂）、氯甲酸丁酯（作为衍生化试剂）和吡啶（作为催化剂）。在微萃取方法中进行了预定的萃取循环后，将得到的混浊溶液暴露于微波辐射下，以增强萃取和衍生化效率。该方法在 EBC 样品中提供了低的检测限（吗啡 2.1 和羟吗啡 1.5ng/mL）和定量限（吗啡 7.2 和羟吗啡 5.2ng/mL）。该方法具有适当的重复性、准确性和稳定性，相对标准偏差分别小于 5.1%、9%和 9%。该方法成功地用于测定成瘾患者 EBC 样品中吗啡和羟吗啡的浓度。
