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Determination of aldosterone in serum by liquid chromatography-tandem mass spectrometry

机译:液相色谱-串联质谱法测定血清中的醛固酮

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Measurement of serum aldosterone is clinically important in the diagnosis of hypertension.)While isotope dilution gas chromatography-mass spectrometry (ID-GC-MS) provides reliable results, it requires derivatization and is lengthy and time-consuming. Detection by liquid chromatography-mass spectrometry (LC-MS) is a potentially superior method. The analysis utilizes 0.5 mL of serum. The samples were extracted with dichloromethane-ether. The extract was evaporated to dryness and aldosterone was analyzed by LC-MS/MS operating in the negative mode ESI after separation on a reversed-phase column. Aldosterone was also measured by RIA. The calibration curves for analysis of serum aldosterone exhibited consistent linearity and reproducibility in the range of 60-3000 pmol/L. Interassay CVs were 4.3-7.5% at aldosterone concentrations of 97-993 pmol/L. The lower limit of quantitation (LOQ) was 30 pmol/L (signal to noise ratio = 10). The mean recovery of the analyte added to serum ranged from 95 to 102%. The regression equation by LC-MS/MS (x) and RIA (y) method was: y = 1.33x + 185 (r = 0.95; n = 124). Sensitivity and specificity of the LC-MS/MS method for serum aldosterone offer advantages over GC-MS by eliminating derivatization. The novel method is rapid, reliable and simple to perform with a routine LC-MS/MS spectrometer. The sensitivity is adequate for patient samples. Aldosterone concentrations reported by nonextraction RIA were consistently higher than those produced by LC-MS/MS. (c) 2007 Elsevier B.V. All rights reserved.
机译:血清醛固酮的测定对高血压的诊断具有重要的临床意义。)虽然同位素稀释气相色谱-质谱法(ID-GC-MS)提供了可靠的结果,但需要衍生化,而且既费时又费时。通过液相色谱-质谱(LC-MS)进行检测是一种潜在的优势方法。分析使用0.5 mL血清。样品用二氯甲烷-乙醚萃取。将萃取液蒸发至干,并在反相柱上分离后,通过以负模式ESI操作的LC-MS / MS分析醛固酮。醛固酮也通过RIA测量。用于分析血清醛固酮的校准曲线在60-3000 pmol / L的范围内表现出一致的线性和重现性。醛固酮浓度为97-993 pmol / L时,测定间CV为4.3-7.5%。定量下限(LOQ)为30 pmol / L(信噪比= 10)。添加到血清中的分析物的平均回收率为95%至102%。通过LC-MS / MS(x)和RIA(y)方法得出的回归方程为:y = 1.33x + 185(r = 0.95; n = 124)。 LC-MS / MS方法对血清醛固酮的敏感性和特异性通过消除衍生作用而提供了优于GC-MS的优势。这种新颖的方法快速,可靠并且使用常规LC-MS / MS光谱仪执行起来简单。灵敏度足以用于患者样品。非萃取RIA报告的醛固酮浓度始终高于LC-MS / MS产生的浓度。 (c)2007 Elsevier B.V.保留所有权利。

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