Volmer D A, Hui J P
Institute for Marine Biosciences, National Research Council, Halifax, Nova Scotia, Canada.
Rapid Commun Mass Spectrom. 1997;11(17):1926-33. doi: 10.1002/(SICI)1097-0231(199711)11:17<1926::AID-RCM97>3.0.CO;2-2.
Solid-phase microextraction combined with fast short-column liquid chromatography/mass spectrometry (SPME/LC/MS) was used for isolating and analysing 11 corticosteroids and 2 steroid conjugates from urine samples. Several SPME parameters such as polarity of fibres, extraction time and effect of ionic strength, were investigated, and their impact on the SPME/LC/MS technique was studied. To demonstrate the potential of the SPME/LC/MS method, its application to the determination of steroids in human urine was investigated. The method was shown to be sensitive with detection limits between 4 and 30 ng/mL and precision between 4.9 and 11.1% RSD through the use of an internal standard technique. The versatility of the method was also exhibited by its excellent linearity in the concentration range of 20 to 20,000 ng/mL in urine for all investigated compounds. A comparison of the SPME/LC/MS method with LC/MS methods utilizing traditional sample preparation techniques, shows that the former offers similar performance in terms of precision, linearity and detection limits, but is clearly easier to use and faster to perform.
采用固相微萃取结合快速短柱液相色谱/质谱联用技术（SPME/LC/MS）从尿液样本中分离并分析11种皮质类固醇和2种类固醇结合物。研究了纤维极性、萃取时间和离子强度影响等几个固相微萃取参数，并研究了它们对SPME/LC/MS技术的影响。为证明SPME/LC/MS方法的潜力，研究了其在测定人尿中类固醇方面的应用。通过使用内标技术，该方法显示出灵敏度，检测限在4至30 ng/mL之间，精密度在4.9%至11.1%相对标准偏差之间。对于所有研究的化合物，该方法在尿液中20至20,000 ng/mL的浓度范围内具有出色的线性，也展示了其通用性。将SPME/LC/MS方法与采用传统样品制备技术的LC/MS方法进行比较，结果表明，前者在精密度、线性和检测限方面具有相似的性能，但使用起来明显更简便，执行速度更快。
