Proton Affinitive Derivatization for Highly Sensitive Determination of Testosterone and Dihydrotestosterone in Saliva Samples by LC-ESI-MS/MS

被引：8

作者：

Ohno, Ken-ichi ^{[1
]}

Hasegawa, Tomomi ^{[1
]}

Tamura, Tomomi ^{[1
]}

Utsumi, Haruka ^{[1
]}

Yamashita, Kouwa ^{[2
]}

机构：

[1] Tohoku Med & Pharmaceut Univ, Fac Pharmaceut Sci, Aoba Ku, 4-1 Komatsushima 4 Chome, Sendai, Miyagi 9818558, Japan

[2] Yokohama Univ Pharm, Totsuka Ku, 601 Matano Cho, Yokohama, Kanagawa 2450066, Japan

来源：

ANALYTICAL SCIENCES | 2018年 / 34卷 / 09期

关键词：

Proton affinitive derivatization; picolinic acid analog; LC-MS/MS; saliva sample; matrix effect; ion suppression; TANDEM MASS-SPECTROMETRY; SERUM TESTOSTERONE; PROSTATE-CANCER; STEROIDS; TISSUE; ASSAY; 5-ALPHA-DIHYDROTESTOSTERONE; METABOLITES; DERIVATIVES; CASTRATION;

D O I：

10.2116/analsci.18SCP08

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

In this study, proton affinitive derivatization using picolinic acid and its analogs (3- and 6-methylpicolinic acid and 5-butylpicolinic acid) with proton affinitive moieties was performed for the highly sensitive determination of testosterone (T) and 5 alpha-dihydrotestosterone (DHT) in saliva by LC-ESI-MS/MS. T and DHT were converted to their corresponding picolinate esters and their chromatographic behavior was investigated with a reversed phase column. The picolinate ester of each steroid exhibited a clear single peak and elution occurred in the following order: picolinate, 3/6-methylpicolinate, and 5-butylpicolinate. Estimation and understanding of the separation and retention time of each picolinate ester was made simple using the develop method. Although the peaks of picolinate and 3/6-methylpicolinate esters were suppressed by interference from the saliva background (matrix effect), the 5-butylpicolinate esters were only marginally affected.

引用

页码：1017 / 1021

页数：5

共 37 条

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