高效液相色谱-示差折光检测法测定磺丁基醚-β-环糊精的含量
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摘要
目的建立辅料SBE_7-β-CD的含量测定方法。方法采用高效液相凝胶色谱法。Phenomenex PolySep-GFC-P3000凝胶柱(7. 8 mm×30 cm),柱温35℃;示差折光检测器,检测温度35℃;流动相:乙腈-0. 1 mol/L硝酸钾水溶液(35∶65),进样量10μl,流速1. 0 ml/min。结果 SBE_7-β-CD的保留时间为6. 8 min,主峰与相邻杂质峰分离度均不小于1. 94;方法的检测限为0. 32μg,定量限为0. 48μg; SBE_7-β-CD在0. 498 5～1. 495 mg/ml范围内线性关系良好(r=0. 999 8);方法精密度(n=6)的RSD为1. 4%;平均回收率(n=6)的平均值为98. 0%,RSD为1. 3%; 6批样品的含量为95. 8%～99. 3%。结论该方法准确度和重复性良好,适合SBE_7-β-CD的含量测定,为SBE_7-β-CD质量控制标准的建立奠定了基础。
Objective To develop a method for the determination of SBE_7-β-CD. Methods An HPLC method was employed. The sample was separated on a Phenomenex PolySep-GFC-P3000 column( 7. 8 mm× 30 cm) at35 ℃. A refractive index detector was used for the detection,and the detective temperature was 35 ℃. The mobile phase was a mixture of acetonitrile-0. 1 mol/L potassiumnitrate aqueous solution( 35∶ 65) at a flowrate of 1. 0 ml/min,and injection size was 10 μl. Results The retention time of SBE_7-β-CD was 6. 8 min. The resolutions of sample and impurities were no less than 1. 94; LOD and LOQ of this method were 0. 32 μg and 0. 48 μg; there was a good linear relationship of SBE_7-β-CD at the range of 0. 498 5 ～ 1. 495 mg/ml( r = 0. 999 8); the precision of method( n = 6)was 1. 4%; the average of recovery was 98. 0% and RSD was 1. 3%; the content of 6 batches of samples was at the range of 95. 8% ～ 99. 3%. Conclusion This method can be used for the determination of SBE_7-β-CD for its accuracy and repeatability,which builds a solid foundation for the establishment of the quality standard of SBE_7-β-CD.
Objective To develop a method for the determination of SBE_7-β-CD. Methods An HPLC method was employed. The sample was separated on a Phenomenex PolySep-GFC-P3000 column( 7. 8 mm× 30 cm) at35 ℃. A refractive index detector was used for the detection,and the detective temperature was 35 ℃. The mobile phase was a mixture of acetonitrile-0. 1 mol/L potassiumnitrate aqueous solution( 35∶ 65) at a flowrate of 1. 0 ml/min,and injection size was 10 μl. Results The retention time of SBE_7-β-CD was 6. 8 min. The resolutions of sample and impurities were no less than 1. 94; LOD and LOQ of this method were 0. 32 μg and 0. 48 μg; there was a good linear relationship of SBE_7-β-CD at the range of 0. 498 5 ～ 1. 495 mg/ml( r = 0. 999 8); the precision of method( n = 6)was 1. 4%; the average of recovery was 98. 0% and RSD was 1. 3%; the content of 6 batches of samples was at the range of 95. 8% ～ 99. 3%. Conclusion This method can be used for the determination of SBE_7-β-CD for its accuracy and repeatability,which builds a solid foundation for the establishment of the quality standard of SBE_7-β-CD.
引文
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[6]王钊,王欣,杨静,等.磺丁基-β-环糊精与齐墩果酸的热力学稳定性研究[J].中国药师,2013,16(5):635-638.
[2]林玉龙,吴海燕,郭伟,等.磺丁基醚-β-环糊精对不同晶型阿折地平的包合作用[J].中国医院药学杂志,2015,35(22):2000-2004.
[3] Luke DR,Tomaszewski K,Damle B,et al. Review of the basic and clinical pharmacology of sulfobutylether-beta-cyclodextrin(SBECD)[J]. J Pharm Sci,2010,99(8):3291-3301.
[4]王彦竹,宋丽明,张赫然,等.β-环糊精及其衍生物在药学中的应用进展[J].中国药房,2014,25(33):3149-3152.
[5]杨学敏,杨波,廖霞俐,等.不同取代度磺丁基醚-β-环糊精的合成工艺研究[J].化学世界,2013,54(2):110-113.
[6]王钊,王欣,杨静,等.磺丁基-β-环糊精与齐墩果酸的热力学稳定性研究[J].中国药师,2013,16(5):635-638.