Weber C, Beetens J, De Clerck F, Tegtmeier F
Janssen Research Foundation, Neuss, Germany.
J Chromatogr. 1992 May 20;577(1):1-7. doi: 10.1016/0378-4347(92)80592-e.
The extension of a method for the determination of thromboxane B2 (TxB2), 2,3-dinor-TxB2, 6-keto-prostaglandin F1 alpha (6-keto-PGF1 alpha) and 2,3-dinor-6-keto-PGF1 alpha to quantify 11-dehydro-TxB2 in the same urinary sample is described. After phenylboronic acid and C18 column chromatography, 11-dehydro-TxB2, which is present in urine as the lactone and its corresponding hydroxy acid, was quantitatively converted into its lactone form for a thin-layer purification step and pentafluorobenzyl esterification. Quantification of eicosanoids was achieved by analysing their trimethylsilyl ethers with gas chromatography and negative-ion chemical ionization mass spectrometry. The overall recovery from urine for tritiated 11-dehydro-TxB2 was 80%. The detection limit was 10 pg/ml. The method was applied to the determination of these eicosanoids in volunteers and in patients suffering from acute myocardial infarction.
本文描述了一种测定血栓素B2（TxB2）、2,3-二去甲-TxB2、6-酮-前列腺素F1α（6-酮-PGF1α）和2,3-二去甲-6-酮-PGF1α的方法扩展，用于在同一尿液样本中定量11-脱氢-TxB2。经过苯基硼酸和C18柱色谱法后，尿液中以内酯及其相应羟酸形式存在的11-脱氢-TxB2被定量转化为其内酯形式，用于薄层纯化步骤和五氟苄基酯化。通过气相色谱法和负离子化学电离质谱法分析其三甲硅烷基醚来实现类花生酸的定量。氚标记的11-脱氢-TxB2从尿液中的总回收率为80%。检测限为10 pg/ml。该方法应用于志愿者和急性心肌梗死患者中这些类花生酸的测定。
