Sakamoto Miho, Kishimoto Kiyoko, Saito Yuri, Suzuki Ikuo, Moriyasu Takako
Tokyo Metropolitan Institute of Public Health, Department of Pharmaceutical Sciences, Tokyo, Japan.
Chirality. 2016 Mar;28(3):204-8. doi: 10.1002/chir.22570. Epub 2016 Jan 15.
A direct chiral liquid chromatography-circular dichroism (LC-CD) method was developed for the simple and rapid identification of N-octylnortadalafil [(6R, 12aR)-6-(1,3-benzodioxol-5-yl)-2-octyl-2,3,6,7,12,12a-hexahydropyrazino[1',2':1,6]pyrido[3,4-b]indole-1,4-dione; RR-OTDF] and its stereoisomers in dietary supplements. Samples were extracted with methanol. Compounds were then separated by chiral LC-CD using Chiralcel OD-RH (4.6 × 150 mm, 5 µm) with 5 mM ammonium formate (pH 3)/0.1% formic acid in acetonitrile (95:5, v/v) mixture solution (mobile phase A) and 0.1% formic acid in acetonitrile (mobile phase B). The isocratic elution used was mobile phase A / mobile phase B (3:7, v/v) at a flow rate of 1 ml/min. The column temperature was held at 30°C. RR-OTDF and its stereoisomers were separated within 20 min with the resolution factors being over 2.0. Using this method, RR-OTDF and (6R, 12aS)-6-(1,3-benzodioxol-5-yl)-2-octyl-2,3,6,7,12,12a-hexahydropyrazino[1',2':1,6]pyrido[3,4-b]indole-1,4-dione were detected in a dietary supplement.
开发了一种直接手性液相色谱 - 圆二色光谱法（LC - CD），用于简单快速地鉴定膳食补充剂中的N - 辛基去甲他达拉非[（6R，12aR）-6 - （1,3 - 苯并二氧杂环戊烯 - 5 - 基）-2 - 辛基 - 2,3,6,7,12,12a - 六氢吡嗪并[1'，2'：1,6]吡啶并[3,4 - b]吲哚 - 1,4 - 二酮；RR - OTDF]及其立体异构体。样品用甲醇萃取。然后使用Chiralcel OD - RH（4.6×150 mm，5 µm）通过手性LC - CD分离化合物，流动相A为5 mM甲酸铵（pH 3）/ 0.1％甲酸的乙腈（95：5，v / v）混合溶液，流动相B为乙腈中的0.1％甲酸。所采用的等度洗脱为流动相A /流动相B（3：7，v / v），流速为1 ml / min。柱温保持在30°C。RR - OTDF及其立体异构体在20分钟内分离，分离度因子超过2.0。使用该方法，在一种膳食补充剂中检测到了RR - OTDF和（6R，12aS）-6 - （1,3 - 苯并二氧杂环戊烯 - 5 - 基）-2 - 辛基 - 2,3,6,7,12,12a - 六氢吡嗪并[1'，2'：1,6]吡啶并[3,4 - b]吲哚 - 1,4 - 二酮。
