Fryirs B, Woodhouse A, Huang J L, Dawson M, Mather L E
Department of Anaesthesia and Pain Management, University of Sydney, Royal North Shore Hospital, St Leonards, NSW, Australia.
J Chromatogr B Biomed Sci Appl. 1997 Jan 10;688(1):79-85. doi: 10.1016/s0378-4347(97)88058-9.
A method was devised to determine fentanyl plasma concentrations by GC-MS using selected-ion monitoring (SIM) with sufentanil as internal standard. This was compared with a commonly used commercial radioimmunoassay (RIA). Sample preparation for GC-MS involved basification of plasma then extraction using n-butyl chloride followed by concentration to dryness and reconstitution in toluene for chromatography. Using 1-ml plasma samples, the estimated limit of detection of fentanyl was 20 pg/ml. Blood samples for pharmacokinetic studies were split and assayed by GC-MS and RIA which had a limit of detection of 200 pg/ml. Pearson's r (r - 0.80, p < 0.0001) indicated the methods were highly correlated at all plasma concentrations. Owing to the greater sensitivity of the method, GC-MS is recommended over RIA for subnanogram determination of fentanyl in plasma.
设计了一种采用气相色谱 - 质谱联用(GC-MS)并以舒芬太尼作为内标通过选择离子监测(SIM)来测定芬太尼血浆浓度的方法。将其与常用的商业放射免疫分析法(RIA)进行比较。GC-MS的样品制备包括将血浆碱化,然后用正丁基氯萃取,接着浓缩至干并在甲苯中复溶用于色谱分析。使用1毫升血浆样品时,芬太尼的估计检测限为20皮克/毫升。用于药代动力学研究的血样被分成两份,分别用GC-MS和检测限为200皮克/毫升的RIA进行测定。皮尔逊相关系数r(r = 0.80,p < 0.0001)表明这两种方法在所有血浆浓度下都具有高度相关性。由于该方法具有更高的灵敏度,因此对于血浆中亚纳克级芬太尼的测定,推荐使用GC-MS而非RIA。