以[¹⁸O]前列腺素B₁为内标，采用气相色谱/选择离子监测法微量测定人血浆中的前列腺素B₁。

Microdetermination of the prostaglandin B1 in human plasma by gas chromatography/selected ion monitoring using [18O]prostaglandin B1 as an internal standard.

作者信息

Hishinuma T, Nakamura H, Itoh K, Ohyama Y, Ishibashi M, Mizugaki M

机构信息

Department of Pharmaceutical Sciences, Tokohu University Hospital, Sendai, Japan.

出版信息

Prostaglandins. 1995 Apr;49(4):239-46. doi: 10.1016/0090-6980(95)00016-4.

DOI:10.1016/0090-6980(95)00016-4

PMID:7667505

Abstract

We devised a simple and effective purification for the microdetermination of prostaglandin B1 (PGB1), a metabolite of PGE1. [18O]PGB1 was synthesized by the repeated base-catalyzed hydrolysis of methyl ester derivatives in H(2)18O, to obtain an internal standard for the gas chromatography/selected ion monitoring (GC/SIM) of PGB1. The methyl ester-methoxime-dimethylisopropylsilyl ether derivative was prepared, then GC/SIM was carried out by monitoring the ion at m/z 448.3 for PGB1 and that at m/z 452.3 for internal standard. A good linear response over the range of 10 pg to 100 ng was demonstrated. We detected PGB1 to a level of about 40 pg/mL in human plasma. This method can be used to determine PGB1 in biological samples.

摘要

我们设计了一种简单有效的纯化方法用于微量测定前列腺素B1（PGB1），它是前列腺素E1（PGE1）的一种代谢产物。通过在H₂¹⁸O中对甲酯衍生物进行反复碱催化水解来合成[¹⁸O]PGB1，以获得用于PGB1气相色谱/选择离子监测（GC/SIM）的内标。制备了甲酯-甲氧肟-二甲基异丙基硅醚衍生物，然后通过监测PGB1的m/z 448.3离子和内标的m/z 452.3离子进行GC/SIM。在10 pg至100 ng范围内显示出良好的线性响应。我们在人血浆中检测到PGB1的水平约为40 pg/mL。该方法可用于测定生物样品中的PGB1。