Xu X, Bartlett M G, Stewart J T
Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, University of Georgia, Athens, Georgia 30602, USA.
J Mass Spectrom. 2000 Nov;35(11):1329-34. doi: 10.1002/1096-9888(200011)35:11<1329::AID-JMS67>3.0.CO;2-G.
Ondansetron and its hydroxylated metabolites were determined in human serum using solid-phase extraction (SPE) and liquid chromatography/positive ion electrospray tandem mass spectrometry. Pyrimethamine was used as the internal standard. The analytes were eluted from the SPE cartridge using 2 x 1 ml of methanol containing 0.5% triethylamine, evaporated under vacuum and the residue was reconstituted in the mobile phase. The liquid chromatographic separation was achieved on a silica column using a mobile phase of aqueous 20 mM ammonium acetate (pH 4.7)-acetonitrile (85 : 15, v/v) at a flow-rate of 0.4 ml min(-1). The method was linear over the range 1-500 ng ml(-1) for ondansetron and each of the metabolites in human serum. The intra-day accuracy was better than 9.1% and the precision was <10.3%; the inter-day accuracy was better than 9.5% and the precision was <12.6%. The limit of detection was 250 pg ml(-1) based on a signal-to-noise ratio of 3. The absolute recovery from serum for all analytes was >90%.
采用固相萃取（SPE）和液相色谱/正离子电喷雾串联质谱法测定人血清中的昂丹司琼及其羟基化代谢产物。以乙胺嘧啶作为内标。使用2×1ml含0.5%三乙胺的甲醇从SPE小柱上洗脱分析物，真空蒸发后，残渣用流动相复溶。在硅胶柱上进行液相色谱分离，流动相为20mM醋酸铵水溶液（pH 4.7）-乙腈（85∶15，v/v），流速为0.4ml min⁻¹。该方法在人血清中昂丹司琼及其各代谢产物1-500ng ml⁻¹范围内呈线性。日内准确度优于9.1%，精密度<10.3%；日间准确度优于9.5%，精密度<12.6%。基于3的信噪比，检测限为250pg ml⁻¹。所有分析物从血清中的绝对回收率>90%。
