QNMR法测定片剂中维生素B_6的含量
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摘要
建立核磁共振波谱法测定维生素B_6含量的方法:在溶剂为D2O、内标为顺丁烯二酸、脉冲序列为zg 30、采样温度为298 K、延迟时间为20 s、采样次数为16次条件下,使用核磁共振波谱仪(AVANCEⅢ)采集样品的1H-NMR谱.结果:供试片剂中维生素B_6平均含量为15. 29%,RSD=2. 4%,平均回收率为99. 39%;平均每片含量为9. 327 mg,在药典规定的标示范围内.结论:核磁共振波谱法测定维生素B_6含量的方法简便,准确度高.
To establish nuclear magnetic resonance(NMR) method for content determination of vitamin B_6,1H-NMR spectra were obtained with a Bruker 400 MHz spectrometer(AVANCEⅢ) at 298 K. For each sample,16 times of scans were recorded with the following parameters: the pulse sequence zg 30,delayed time of 20 s. Vitamin B_6 was mixed with maleic acid as internal standard in D_2O. Results show as follows:the average content of vitamin B_6 and RSD are 15. 29% and 2. 4% respectively; the average recovery is99. 39%; the average content of vitamin B_6 in each tablet is 9. 327 mg within the scope specified in the pharmacopoeia. The conclusion is that this method is simple and accurate for quantitative analysis of vitamin B_6 in tablets.
To establish nuclear magnetic resonance(NMR) method for content determination of vitamin B_6,1H-NMR spectra were obtained with a Bruker 400 MHz spectrometer(AVANCEⅢ) at 298 K. For each sample,16 times of scans were recorded with the following parameters: the pulse sequence zg 30,delayed time of 20 s. Vitamin B_6 was mixed with maleic acid as internal standard in D_2O. Results show as follows:the average content of vitamin B_6 and RSD are 15. 29% and 2. 4% respectively; the average recovery is99. 39%; the average content of vitamin B_6 in each tablet is 9. 327 mg within the scope specified in the pharmacopoeia. The conclusion is that this method is simple and accurate for quantitative analysis of vitamin B_6 in tablets.
引文
[1]黄绿苗.维生素B6的进展性研究[J].医学美学美容(中旬刊),2014(7):607.
[2]沈丽平. HPLC测定维生素B6片含量测定方法的探讨[J].海峡药学,2016,28(2):75-76.
[3]曹高娃,崔毅,张力,等.紫外分光光度法测定维生素B6[J].光谱实验室,2001,18(6):802-803.
[4]HOLZGRABE B,DEUBNER R,SCHOLLMAYER C,et a1. Quantitative NMR spectroscopy-applications in drug analysis[J].J Pharm Biomed Anal,2005,38(1):806-812.
[5]国家药典委员会.中华人民共和国药典(2010年版二部)[M].北京:中国医药科技出版社,2010.
[6]陈春丽,田兰,马晓丽,等.核磁共振内标法测定维生素C片中维生素C的含量[J].中国药房,2010,21(32):3063-3065.
[7]胡敏芳,江明,邱慧,等.维生素B2的NMR含量测定[J].分析测试学报,2013,32(12):1511-1514.
[8]鲁瑞娟,吴崇荣,方萍.核磁共振波谱法测定片剂中维生素B1的含量[J].理化检验(化学分册),2016,52(3):323-327.
[9]郭强胜,刘明珂,禹珊,等.定量核磁共振法同时测定复合维生素B片中B1、B2、烟酰胺和泛酸钙[J].波谱学杂志,2016,33(3):442-451.
[10]张友杰,刘小鹏.药物核磁共振定量分析参数的研究[J].波谱学杂志,2007,24(3):289-295.
[2]沈丽平. HPLC测定维生素B6片含量测定方法的探讨[J].海峡药学,2016,28(2):75-76.
[3]曹高娃,崔毅,张力,等.紫外分光光度法测定维生素B6[J].光谱实验室,2001,18(6):802-803.
[4]HOLZGRABE B,DEUBNER R,SCHOLLMAYER C,et a1. Quantitative NMR spectroscopy-applications in drug analysis[J].J Pharm Biomed Anal,2005,38(1):806-812.
[5]国家药典委员会.中华人民共和国药典(2010年版二部)[M].北京:中国医药科技出版社,2010.
[6]陈春丽,田兰,马晓丽,等.核磁共振内标法测定维生素C片中维生素C的含量[J].中国药房,2010,21(32):3063-3065.
[7]胡敏芳,江明,邱慧,等.维生素B2的NMR含量测定[J].分析测试学报,2013,32(12):1511-1514.
[8]鲁瑞娟,吴崇荣,方萍.核磁共振波谱法测定片剂中维生素B1的含量[J].理化检验(化学分册),2016,52(3):323-327.
[9]郭强胜,刘明珂,禹珊,等.定量核磁共振法同时测定复合维生素B片中B1、B2、烟酰胺和泛酸钙[J].波谱学杂志,2016,33(3):442-451.
[10]张友杰,刘小鹏.药物核磁共振定量分析参数的研究[J].波谱学杂志,2007,24(3):289-295.