Determination of Principal Compound and Related Substances in Raw Material Drug of Menaquinone-7 by UPLC
摘 要
Menaquinone-7原料药在避光条件下经无水乙醇超声溶解后,采用Agilent Eclipse plus C18色谱柱(2.1 mm×50 mm,1.8 μm)分离主成分及有关物质,以甲醇-水(98+2)混合液为流动相,分别在波长246,270 nm处测定主成分及有关物质。Menaquinone-7的线性范围在0.005~0.400 g·L-1内,检出限(3S/N)为0.1 mg·L-1。加标回收率在98.8%~100%之间,测定值的相对标准偏差(n=6)小于1.0%。测得两批Menaquinone-7原料药中主成分的质量分数分别为98.0%,98.2%,单个杂质质量分数小于0.5%,杂质总质量分数小于1.0%。
Abstract
Raw material drug of Menaquinone-7 was dissolved ultrasonically with ethanol in the dark, and then the principal compound and related substances in the sample were separated on an Agilent Eclipse plus C18 chromatographic column (2.1 mm×50 mm, 1.8 μm). The mobile phase was methanol-water (98+2) solution, and the detection wavelengths were 246, 270 nm for the determination of principal compound and related substances, respectively. The linearity range of Menaquinone-7 was 0.005-0.400 g·L-1, with detection limit (3S/N) of 0.1 mg·L-1. Recovery rates obtained by standard addition method were in the range of 98.8%-100% and RSDs (n=6) were less than 1.0%. The contents of the principal compound in 2 batches of Menaquinone-7 raw material drug were 98.0% and 98.2%. The mass fraction of single impurity was less than 0.5%, and the mass fraction of total impurities was less than 1.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201712004
所属栏目 工作简报
基金项目 国家自然科学基金(21562044)
收稿日期 2016/12/10
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备注宋怡(1983-),女,云南昆明人,主管药师,主要从事药品检验研究工作,songyi19830@21cn.com
引用该论文: SONG Yi,KONG Fanjian,LI Yinke,WANG Quan. Determination of Principal Compound and Related Substances in Raw Material Drug of Menaquinone-7 by UPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(12): 1381~1385
宋怡,孔凡建,李银科,王泉. 超高效液相色谱法测定Menaquinone-7原料药主成分及有关物质[J]. 理化检验-化学分册, 2017, 53(12): 1381~1385
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参考文献
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【4】IWAMOTO J, SATO Y, TAKEDA T, et al. High-dose vitamin K supplementation reduces fracture incidence in postmenopausal women:A review of the literature[J]. Nutrition Research, 2009,29(4):221-228.
【5】URANO A, HOTTA M, OHWADA R, et al. Vitamin K deficiency evaluated by serum levels of undercarboxylated osteocalcin in patients with anorexia nervosa with bone loss[J]. Clinical Nutrition, 2014,34(3):443-448.
【6】HAMIDI M S, GAJIC-VELJANOSKI O, CHEUNG A M. Vitamin K and bone health[J]. Journal of Clinical Densitometry, 2013,16(4):409-413.
【7】詹芝娅.凝血/纤溶系统与SIRS、Sepsis[J].黑龙江医药, 2008,21(5):69-71.
【8】XIA J H, MATSUHASHI S, HAMAJIMA H, et al. The role of PKC isoforms in the inhibition of NF-κB activation by vitamin K2 in human hepatocellular carcinoma cells[J]. The Journal of Nutritional Biochemistry, 2012,23(12):1668-1675.
【9】YOSHIJI H, NOGUCHI R, TOYOHARA M, et al. Combination of vitamin K2 and angiotensin-converting enzyme inhibitor ameliorates cumulative recurrence of hepatocellular carcinoma[J]. Journal of Hepatology, 2009,51(2):315-321.
【10】KIELY M, HODGINS S J, MERRIGAN B A, et al. Real-time cell analysis of the inhibitory effect of vitamin K2 on adhesion and proliferation of breast cancercells[J]. Nutrition Research, 2015,35(8):736-743.
【11】朱杰,王中群,王昭军,等.维生素K2抑制血管钙化作用与机制研究进展[J].中华老年心脑血管病杂志, 2016,18(1):94-96.
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【13】GENTILI A, MICCHELI A, TOMAI P, et al. Liquid chromatography-tandem mass spectrometry method for the determination of vitamin K homologues in human milk after overnight cold saponification[J]. Journal of Food Composition and Analysis, 2016,47:21-30.
【14】VIÑAS P, BRAVO-BRAVO M, LÓPEZ-GARCÍA I, et al. Dispersive liquid-liquid microextraction for the determination of vitamins D and K in foods by liquid chromatography with diode-array and atmospheric pressure chemical ionization-mass spectrometry detection[J]. Talanta, 2013,15:806-813.
【15】SUHARA Y, KAMAO M, TSUGAWA N, et al. Method for the determination of vitamin K homologues in human plasma using high-performance liquid chromatography-tandem mass spectrometry[J]. Analytical Chemistry, 2005,77(3):757-763.
【16】JAKOB E, ELMADFA I. Rapid and simple HPLC analysis of vitamin K in food, tissues and blood[J]. Food Chemistry, 2000,68:219-223.
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