贝前列素钠中异构体检测方案(液相色谱柱)

HPLC DATASHEETT器信息网 八号才口又卜十卜中么(日本薬局方記載条件)Beraprost sodium (The Japanese Pharmacopoeia) D111213C 1 Column ： YMC-Pack Pro C18 (5 um，12 nm) 150 X6.0mml.D. Eluent I： methanol/water/acetic acid (60/40/0.1) Flow rate ： 1.2mL/min (adjust the flow rate so that the retention time of the second peak of beraprost is about 27 min) Temperature ：40℃ Detection ： UV at 285 nm Injection ： 15 pL (0.5 mg/mL) (Modified conditions of The Japanese Pharmacopoeia 16th； Isomer ratio) Isomer ratio Dissolve 10 mg of Beraprost Sodium in 5 mL of methanol, and use this solution as the sample solution.Perform the test with 15 mL of the sample solution as directed under Liquid Chromatography <2.01> according to the following conditions, and determine the areas, Aa of the peak which appears at the retention time about 25 minutes, and Ab of the peak which appears at about 27 minutes: Ab/Aa is between 0.90 and 1.10.Operating conditions—    Detector: An ultraviolet absorption photometer (wavelength:285 nm).    Column: A stainless steel column 6 mm in inside diameter and 15 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (5 mm in particle diameter).    Column temperature: A constant temperature of about 40℃.    Mobile phase: A mixture of methanol, water and acetic acid (100) (600:400:1).    Flow rate: Adjust so that the retention time of the second eluting peak of beraprost is about 27 minutes.System suitability—    System performance: When the procedure is run with 15 μL of the sample solution under the above operating conditions, the resolution between the two peaks of beraprost is not less than 1.2.    System repeatability: When the test is repeated 6 times with 15 μL of the sample solution under the above operating conditions, the relative standard deviation of the total area of the two peak of beraprost is not more than 2.0%.