Jedynak Łukasz, Jedynak Maria, Kossykowska Magdalena, Zagrodzka Joanna
Pharmaceutical Research Institute, R&D Analytical Chemistry Department, Rydygiera 8, 01-793 Warsaw, Poland.
Pharmaceutical Research Institute, R&D Analytical Chemistry Department, Rydygiera 8, 01-793 Warsaw, Poland.
J Pharm Biomed Anal. 2017 Feb 20;135:116-125. doi: 10.1016/j.jpba.2016.11.052. Epub 2016 Dec 10.
An HPLC method with UV detection and separation with the use of a C30 reversed phase analytical column for the determination of chemical purity and assay of menaquinone-7 (MK7) in one chromatographic run was developed. The method is superior to the methods published in the USP Monograph in terms of selectivity, sensitivity and accuracy, as well as time, solvent and sample consumption. The developed methodology was applied to MK7 samples of active pharmaceutical ingredient (API) purity, MK7 samples of lower quality and crude MK7 samples before purification. The comparison of the results revealed that the use of USP methodology could lead to serious overestimation (up to a few percent) of both purity and MK7 assay in menaquinone-7 samples.
开发了一种采用紫外检测、使用C30反相分析柱进行分离的高效液相色谱法，可在一次色谱运行中测定甲萘醌-7（MK7）的化学纯度和含量。该方法在选择性、灵敏度和准确性方面，以及时间、溶剂和样品消耗方面均优于美国药典专论中公布的方法。所开发的方法应用于活性药物成分（API）纯度的MK7样品、质量较低的MK7样品以及纯化前的粗MK7样品。结果比较表明，使用美国药典方法可能导致甲萘醌-7样品的纯度和MK7含量严重高估（高达百分之几）。
