Shimada K, Mitamura K, Nakatani I
Faculty of Pharmaceutical Sciences, Kanazawa University, Japan.
J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):348-54. doi: 10.1016/s0378-4347(96)00377-5.
The characterization of vitamin D2 3-glucuronide, 25-hydroxyvitamin D2 3-glucuronide and 25-hydroxyvitamin D2 25-glucuronide, biliary metabolites obtained from rats dosed with vitamin D2 and 25-hydroxyvitamin D2 per os, was carried out using HPLC-atmospheric pressure chemical ionization (APCI)-MS. The glucuronide obtained from bile specimens was identified by comparison of its chromatographic behaviour with an authentic sample using HPLC-APCI-MS operating in the negative-ion mode. Methylation of the respective fraction with diazomethane gave the methyl ester, which was also confirmed by HPLC-APCI-MS operating in the positive-ion mode. The (M-H)- and (M + NH4)+ ions were monitored in the selected-ion monitoring mode.
对经口给予维生素D2和25-羟基维生素D2的大鼠胆汁中获得的胆代谢产物维生素D2 3-葡萄糖醛酸苷、25-羟基维生素D2 3-葡萄糖醛酸苷和25-羟基维生素D2 25-葡萄糖醛酸苷进行了表征，采用高效液相色谱-大气压化学电离（APCI）-质谱法。通过在负离子模式下运行的高效液相色谱-大气压化学电离质谱法，将胆汁标本中获得的葡萄糖醛酸苷与其真实样品的色谱行为进行比较来鉴定。用重氮甲烷对各部分进行甲基化得到甲酯，这也通过在正离子模式下运行的高效液相色谱-大气压化学电离质谱法得到证实。在选择离子监测模式下监测（M-H）-和（M+NH4）+离子。
