RP-HPLC测定4,5,2′-三吗啉酰氧基-2,5'-二氯二苯甲酮原料药的含量及有关物质
|
摘要
目的建立测定原料药4,5,2′-三吗啉酰氧基-2,5'-二氯二苯甲酮(LF1)的含量及有关物质的RP-HPLC方法。方法采用Diamonsil C_(18)(250 mm×4.6 mm,5μm)色谱柱,乙腈-磷酸水(60:40,pH3.0)为流动相,检测波长230 nm,体积流量1 mL/min,柱温25℃。结果主峰与杂质峰分离良好,LF1和杂质A分别在质量浓度1.0～100(r=0.999 8)和0.2～2.4 mg/L(r=0.999 6)线性关系良好,最低检测限分别为1和2 ng/mL,平均回收率分别为100.7%和102.0%。结论本法简便、快速、准确,可用于LF1原料药的含量及有关物质的测定。
Objective This paper aims to establish a RP-HPLC method to determine the content of 4,5,2'-trimorpholinyl acyloxy-2,5'-dichlorobenzophenone(LF1) and its related substances.Methods The HPLC method was explored on Diamonsil C_(18)(250 mm × 4.6 mm, 5 μm) with acetonitrile-phosphoric acid water(60:40, pH 3.0) as the mobile phase. The detection wavelength was 230 nm, the flow rate was 1 mL/min and the column temperature was 25 ℃. Results The LF1 was well separated from the impurities,respectively. The calibration curves of LF1 and impurity A showed good linear relationship within 1.0—100(r = 0.999 8) and 0.2—2.4 mg/L(r = 0.999 6), The lowest limit of detection for LF1 and impurity A were 1 and 2 ng/mL, and the average recoveries were100.7% and 102.0%, respectively.Conclusion The established HPLC method is simple, rapid and accurate, and can be used for the determination of LF1 and its related substances.
Objective This paper aims to establish a RP-HPLC method to determine the content of 4,5,2'-trimorpholinyl acyloxy-2,5'-dichlorobenzophenone(LF1) and its related substances.Methods The HPLC method was explored on Diamonsil C_(18)(250 mm × 4.6 mm, 5 μm) with acetonitrile-phosphoric acid water(60:40, pH 3.0) as the mobile phase. The detection wavelength was 230 nm, the flow rate was 1 mL/min and the column temperature was 25 ℃. Results The LF1 was well separated from the impurities,respectively. The calibration curves of LF1 and impurity A showed good linear relationship within 1.0—100(r = 0.999 8) and 0.2—2.4 mg/L(r = 0.999 6), The lowest limit of detection for LF1 and impurity A were 1 and 2 ng/mL, and the average recoveries were100.7% and 102.0%, respectively.Conclusion The established HPLC method is simple, rapid and accurate, and can be used for the determination of LF1 and its related substances.
引文
[1] Wei Y X, Xu Z H. Study on antioxidant activity of high molecular weight fucoidan in brown algae[J]. Chin Herb Med, 2003, 34(4):317-319.
[2] Li K, Li X M, Ji N Y, et al. Natural bromophenols from the marine red alga Polysiphoniaurceolata(Rhodomelaceae):Structural elucidation and DPPH radical-scavenging activity[J]. Bioorg Med Chem, 2007,15(21):6627-6631.
[3] Wang B G, Zhang W W, Duan X J, et al. In vitro antioxidative activities of extract and semi-purified fractions of the marine red alga, Rhodomelaconfervoides(Rhodomelaceae)[J]. Food Chem, 2009, 113(4):1101-1105.
[4] Katsui N, Suzuki Y, Kitamura S, et al. 5, 6-Dibromoprotocatechualdehyde and 2, 3-dibromo-4, 5-dihydroxybenzyl methyl ether:New dibromophenols from rhodomelalarix[J]. Tetrahedron, 1967, 23(3):1185-1188.
[5] Choi J S, Park H J, Jung H A, et al. A cyclohexanonyl bromophenol from the red alga Symphyocladialatiuscula[J]. J Nat Prod, 2000, 63(12):1705-1706.
[6] Duan X J, Zhang W W, Li X M, et al. Evaluation of antioxidant property of extract and fractions obtained from a red alga, Polysiphoniaurceolata[J]. Food Chemistry, 2006, 95(1):37-43.
[7] Zhao W Y, Feng X E, Ban S R, et al. Synthesis and biological activity of halophenols as potent antioxidant and cytoprotective agents[J]. Bioorg Med Chem Lett,2010, 20(14):4132-4134.
[8]李青山,张圆琳,冯秀娥.氮甲酰氧基取代的氯代二苯甲酮类衍生物[P].中国:ZL201610278055.8, 2017-8-25.
[9]李青山,冯秀娥,常熔熔.两种卤酚化合物在制备抗Ⅱ型糖尿病肾病药物中的应用[P].中国:201610278158.4,2016-4-29.
[10]王文清,高春丽,蔡钰.高效液相色谱法测定对羟基苯甲酸甲酯的含量及有关物质[J].中国药师, 2009, 12(1):70-72.
[11]崔红霞,霍艳双,李清,等.反相高效液相色谱法测定WF-208的含量和有关物质[J].中国新药杂志, 2012(17):2069-2071.
[2] Li K, Li X M, Ji N Y, et al. Natural bromophenols from the marine red alga Polysiphoniaurceolata(Rhodomelaceae):Structural elucidation and DPPH radical-scavenging activity[J]. Bioorg Med Chem, 2007,15(21):6627-6631.
[3] Wang B G, Zhang W W, Duan X J, et al. In vitro antioxidative activities of extract and semi-purified fractions of the marine red alga, Rhodomelaconfervoides(Rhodomelaceae)[J]. Food Chem, 2009, 113(4):1101-1105.
[4] Katsui N, Suzuki Y, Kitamura S, et al. 5, 6-Dibromoprotocatechualdehyde and 2, 3-dibromo-4, 5-dihydroxybenzyl methyl ether:New dibromophenols from rhodomelalarix[J]. Tetrahedron, 1967, 23(3):1185-1188.
[5] Choi J S, Park H J, Jung H A, et al. A cyclohexanonyl bromophenol from the red alga Symphyocladialatiuscula[J]. J Nat Prod, 2000, 63(12):1705-1706.
[6] Duan X J, Zhang W W, Li X M, et al. Evaluation of antioxidant property of extract and fractions obtained from a red alga, Polysiphoniaurceolata[J]. Food Chemistry, 2006, 95(1):37-43.
[7] Zhao W Y, Feng X E, Ban S R, et al. Synthesis and biological activity of halophenols as potent antioxidant and cytoprotective agents[J]. Bioorg Med Chem Lett,2010, 20(14):4132-4134.
[8]李青山,张圆琳,冯秀娥.氮甲酰氧基取代的氯代二苯甲酮类衍生物[P].中国:ZL201610278055.8, 2017-8-25.
[9]李青山,冯秀娥,常熔熔.两种卤酚化合物在制备抗Ⅱ型糖尿病肾病药物中的应用[P].中国:201610278158.4,2016-4-29.
[10]王文清,高春丽,蔡钰.高效液相色谱法测定对羟基苯甲酸甲酯的含量及有关物质[J].中国药师, 2009, 12(1):70-72.
[11]崔红霞,霍艳双,李清,等.反相高效液相色谱法测定WF-208的含量和有关物质[J].中国新药杂志, 2012(17):2069-2071.