超高效液相色谱-串联质谱法同时测定人尿中雄激素和前列腺素。

PubMed ID
G H
发表日期 2019年Mar月

原始出处 色谱杂志。B、 生物医学和生命科学中的分析技术
Journal of chromatography. B, Analytical technologies in the biomedical and life sciences
作者 Im  Eunju  Lew  Bark Lynn  Lee  Mi Yeon  Lee  Jeongae  Paeng  Ki Jung  Chung  Bong Chul 

文献标题 超高效液相色谱-串联质谱法同时测定人尿中雄激素和前列腺素。
Simultaneous determination of androgens and prostaglandins in human urine using ultra-high-performance liquid chromatography-tandem mass spectrometry.
Simultaneous determination of androgens and prostaglandins in human urine using ultra-high-performance liquid chromatography-tandem mass spectrometry.

文献摘要

建立了一种同时测定雄激素和前列腺素的超高效液相色谱-串联质谱定量分析方法。在样品制备过程中,固相萃取和液-液萃取相结合。β-葡萄糖醛酸酶/芳基磺酸酶也用于酶水解步骤。以2-肼吡啶为衍生试剂,在同一电离模式下同时测定雄激素和前列腺素。在22小时的运行时间内,采用正离子模式下的多反应监测对所有分析物进行分离和测量 方法经验证,总回收率为81.0-102.9%,定量限为0.01-2% 日内准确率为6.5%~14.3%,精密度为77.1%~106.8%。日间准确率为8.9%~18.2%,精密度为89.9%~101.4%。线性关系用相关系数表示,相关系数>0.99。本文提出的方法通过治疗男性型秃发患者和正常对照组之间尿雄激素和前列腺素水平的差异来研究一年非那雄胺治疗的效果。服用非那雄胺后两组尿雄激素和前列腺素水平无显著性差异。结果证实,非那雄胺影响雄激素和PGs与头发再生和生长长度有关,一年的非那雄胺治疗MPB是有效的。基于质谱的定量分析方法用于男性型秃发的研究,对于评估与各种炎症性疾病代谢相关的雄激素和前列腺素也有很大的潜力。


A simultaneous quantitative profiling method for androgens and prostaglandins using ultra-high-performance liquid chromatography-tandem mass spectrometry was developed and validated to evaluate urinary androgen and prostaglandin levels. Solid-phase extraction and liquid-liquid extraction steps were combined during the sample preparation. β-Glucuronidase/arylsulfatase was also used in the enzyme hydrolysis step. Chemical derivatization was performed using 2-hydrazinopyridine for simultaneous determination of androgen and prostaglandin in the same ionization mode. The analytes were all separated and measured using multiple reaction monitoring in the positive ion mode within a run time of 22 min. The method was validated, achieving overall recoveries ranging from 81.0 to 102.9% with limits of quantification ranging from 0.01 to 2 ng/mL. The intra-day accuracy and precision ranged from 6.5 to 14.3% and from 77.1 to 106.8%, respectively. The inter-day accuracy and precision ranged from 8.9 to 18.2% and 89.9 to 101.4%, respectively. The linearity was expressed using the correlation coefficient, which was >0.99. The method developed herein was used to investigate the effects of a one-year finasteride treatment through differences in urinary androgen and prostaglandin levels between treated male pattern baldness patients and normal controls. The urinary androgen and prostaglandin levels were not significantly different between the two groups because of the administration of finasteride. The results confirmed that finasteride affects androgens and PGs related to hair regrowth and growth length, and a one-year finasteride treatment is effective for MPB. The mass spectrometry-based quantitative profiling method used herein for the investigation of male pattern baldness also holds great potential for the evaluation of androgens and prostaglandins associated with the metabolism of various inflammatory diseases.

A simultaneous quantitative profiling method for androgens and prostaglandins using ultra-high-performance liquid chromatography-tandem mass spectrometry was developed and validated to evaluate urinary androgen and prostaglandin levels. Solid-phase extraction and liquid-liquid extraction steps were combined during the sample preparation. β-Glucuronidase/arylsulfatase was also used in the enzyme hydrolysis step. Chemical derivatization was performed using 2-hydrazinopyridine for simultaneous determination of androgen and prostaglandin in the same ionization mode. The analytes were all separated and measured using multiple reaction monitoring in the positive ion mode within a run time of 22 min. The method was validated, achieving overall recoveries ranging from 81.0 to 102.9% with limits of quantification ranging from 0.01 to 2 ng/mL. The intra-day accuracy and precision ranged from 6.5 to 14.3% and from 77.1 to 106.8%, respectively. The inter-day accuracy and precision ranged from 8.9 to 18.2% and 89.9 to 101.4%, respectively. The linearity was expressed using the correlation coefficient, which was >0.99. The method developed herein was used to investigate the effects of a one-year finasteride treatment through differences in urinary androgen and prostaglandin levels between treated male pattern baldness patients and normal controls. The urinary androgen and prostaglandin levels were not significantly different between the two groups because of the administration of finasteride. The results confirmed that finasteride affects androgens and PGs related to hair regrowth and growth length, and a one-year finasteride treatment is effective for MPB. The mass spectrometry-based quantitative profiling method used herein for the investigation of male pattern baldness also holds great potential for the evaluation of androgens and prostaglandins associated with the metabolism of various inflammatory diseases.


获取全文 10.1016/j.jchromb.2019.01.022