| 液相色谱-串联质谱联用技术检测人尿中去氨加压素及其在人尿中的消除研究 |
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| 中文摘要:建立了液相色谱-串联质谱（LC-MS/MS）检测人尿中去氨加压素的方法。样品经Waters C18固相萃取净化，Phenomenex Onyx Monolothic C18色谱柱分离，以10 mmol/L甲酸铵水溶液（用甲酸调至pH 35）-乙腈作为流动相进行梯度洗脱，流速为04 mL/min，串联质谱正离子模式电离（ESI+），多反应监测模式（MRM）检测。收集8名志愿者在服用单次单剂量去氨加压素后留取3 d内全部尿液样本，使用建立的方法进行检测并绘制代谢曲线。结果表明：尿中去氨加压素的检出限为02 μg/L；线性范围为05~20 μg/L，相关系数（r2）大于 0997；在低、中、高3个加标浓度下，回收率均高于59%，日内及日间精密度均小于10%，基质效应在20%以内。8名志愿者的阳性尿中去氨加压素浓度峰值在服药后70~150 min之间，最高浓度为02~24 μg/L，检测窗口期最长可至服药后13 h左右。该法对于尿中去氨加压素具有特异性，能显著降低实验时间和成本，完全满足世界反兴奋剂组织对该药物的检测要求。该实验考察了服药后阳性尿中去氨加压素的浓度变化，研究了去氨加压素在人体内的消除情况。 |
| 中文关键词:兴奋剂 液相色谱-串联质谱（LC-MS/MS） 去氨加压素 人尿 消除 |
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| Study on Determination of Desmopressin in Human Urine by LC-MS/MS and Its Elimination |
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| Abstract:A method for the determination of desmopressin in urine by liquid chromatography-tandem mass spectrometry was established.The sample was purified by Waters C18 solid phase extraction，and separated on a Phenomenx Onyx C18 chromatographic column.The analysis on the target compound was performed by MS in positive ion ionization under multiple reaction monitoring（MRM） mode.Total of eight volunteers were invited to reserve their urine samples within 3 d after each took a single-dose of desmopressin.The samples were detected by the established method and the metabolic curves for the analyte were drawn out.Results showed that the limits of detection of the method were 02 μg/L.There were linearities for desmopressin in the range of 05-20 μg/L with correlation coefficients（r2） larger than 0997.The recoveries at three spiked levels of low，medium and high concentrations were all higher than 59%，with the intra day and inter day precisions all less than 10%，and the matrix effects within 20%.The peak concentrations of desmopressin in eight volunteers occurred within 70-150 min after taking the drug，and the highest concentrations were in the range of 02-24 μg/L.The longest detection window period could last for about 13 h.This method is unique for the detection of desmopressin in urine，and fully meets the requirements of the World Anti doping Agency for 2 μg/L concentration of the drug by reducing the experiment time and the experimental cost.This method was used to analyze the positive urine after taking the drug，and the elimination of desmopressin in the human body was also investigated. |
| Key Words:doping control liquid chromatography-tandem mass spectrometry（LC-MS/MS） desmopressin human urine elimination |
| 引用本文：闫宽，董颖，徐友宣，马艳华，张力思，杨志勇，冯飞飞.液相色谱-串联质谱联用技术检测人尿中去氨加压素及其在人尿中的消除研究[J].分析测试学报,2018,37(8):950-954. |
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