Barrett Yu Chen, Akinsanya Billy, Chang Shu-Ying, Vesterqvist Ole
Bristol-Myers Squibb Company, Clinical Discovery, P.O. Box 5400, Princeton, NJ 08543, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Jul 25;821(2):159-65. doi: 10.1016/j.jchromb.2005.04.030.
A sensitive method for quantitation of urinary 6beta-hydroxycortisol (6beta-HC) and cortisol using on-line SPE and LC-MS/MS was developed and validated. Human urine samples were injected directly onto an on-line solid phase extraction apparatus, Prospekt-2, followed by HPLC separation and electrospray triple quadrupole LC-MS/MS detection. The inter-day precision for the 6beta-HC:cortisol ratio was 7-9%. The lower limit of quantitation was 1 and 0.2 ng/mL for 6beta-HC and cortisol, respectively. Using the method we observed a diurnal variation on the 6beta-HC:cortisol ratio in healthy volunteers with the maximal ratio observed in the 2-10 pm urine collection period.
开发并验证了一种使用在线固相萃取（SPE）和液相色谱-串联质谱（LC-MS/MS）定量测定尿中6β-羟基皮质醇（6β-HC）和皮质醇的灵敏方法。将人尿液样本直接注入在线固相萃取装置Prospekt-2，随后进行高效液相色谱（HPLC）分离和电喷雾三重四极杆LC-MS/MS检测。6β-HC与皮质醇比值的日间精密度为7-9%。6β-HC和皮质醇的定量下限分别为1和0.2 ng/mL。使用该方法，我们观察到健康志愿者尿中6β-HC与皮质醇比值存在昼夜变化，在下午2点至10点的尿液收集时段观察到最大比值。
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