液相色谱串联质谱法测定人血清色氨酸及其代谢产物的浓度

发布时间：2018-04-18 09:21

  本文选题：液相色谱串联质谱法 + 色氨酸　； 参考：《中国临床药理学杂志》2016年19期

【摘要】：目的建立人血清中色氨酸、犬尿氨酸、喹啉酸浓度测定的液相色谱串联质谱法。方法以甲醇为提取剂,用蛋白沉淀法。色氨酸、犬尿氨酸以犬尿氨酸-13C4,15N为内标,色谱柱:Eclipse XDB-C18(4.6 mm×150 mm,5μm),流动相为甲醇-水(45∶55,均含5 mmol·L~(-1)甲酸铵-0.1%甲酸);喹啉酸以喹啉酸-d3为内标,色谱柱:Eclipse plus C8柱(4.6 mm×100 mm,3.5μm),流动相:甲醇-水(15∶85,0.75 mmol·L~(-1)甲酸铵-0.4%甲酸);流速:0.5 m L·min-1,柱温:35℃;电喷雾离子源,以正离子多反应监测。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应和稳定性。结果色氨酸、犬尿氨酸、喹啉酸的线性范围分别为1000~3×104,100~3000,10~300 ng·m L~(-1);定量下限分别为1000,100,10 ng·m L~(-1);平均回收率均在80%以上,日内、日间精密度RSD均小于15%。结论本方法操作简便,灵敏度高,分析快速,符合生物样品分析要求,适用于人血清中色氨酸及其代谢产物的浓度测定。
[Abstract]:Objective to establish a liquid chromatography-tandem mass spectrometry (LC-MS) method for the determination of tryptophan, canine uric acid and quinolinic acid in human serum.Methods methanol was used as extractant and protein precipitation method was used.Tryptophan, canine uric acid and quinolinic acid were used as internal standard. The chromatographic column was: eclipse XDB-C18(4.6 mm 脳 150mm ~ 5 渭 m, mobile phase was methanol-water 45: 55, both contained 5 mmol L ~ (-1) ammonium formate -0.1% formic acid, and quinolinic acid was quinolinic acid _ d _ 3 as internal standard.The chromatographic column: eclipse plus C8 column was 4.6 mm 脳 100mm ~ 3. 5 渭 m ~ (-1), mobile phase: methanol-water 15: 85 ~ 0.75 mmol / L ~ (-1) ammonium formate -0.4% formate; flow rate: 0.5 mL 路min ~ (-1), column temperature: 35 鈩，

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