定量核磁共振波谱法测定片剂中吡罗昔康
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摘要
建立了定量核磁共振波谱法测定片剂中吡罗昔康含量的方法。以咖啡因为内标,选择~1H-NM R的脉冲程序,延迟时间为12 s,采样次数为32次,以吡罗昔康中δ2.969的峰为定量峰,咖啡因中δ4.006的峰为内标定量峰。吡罗昔康与内标咖啡因的质量比在0.25~6.0的范围内具有良好的线性关系,线性相关系数为0.9993。吡罗昔康片的加标回收率为97.7%~101.0%,相对标准偏差为0.42%~1.2%。方法可用于吡罗昔康片剂含量的测定。
A quantitative nuclear magnetic resonance spectroscopy( q NMR) method was established for the determination of piroxicam in piroxicam tablets. Piroxicam and caffeine as internal standard were dissolved in deuterated chloroform and then analyzed by ~1H-NMR. The delay time and number of scans were set as 12 s and 32,respectively. The peak of δ 2. 696 of piroxicam and δ 4. 006 of caffeine were selected as quantitative peak and internal standard peak,respectively. In the mass ratio range of 0. 25 ~ 6. 0,a good linear relationship was established with correlative coefficient( r~2) of 0. 9993 for piroxicam. The average recovery and relative standard deviation for piroxicam tablets were 97. 7% ~101. 0% and 0. 42% ~ 1. 2%,respectively. The content of piroxicam in tablets was in consistence with the labeled amount. The results showed that the q NMR method was reliable and could be applied to the measurement of piroxicam in sustained tablets.
A quantitative nuclear magnetic resonance spectroscopy( q NMR) method was established for the determination of piroxicam in piroxicam tablets. Piroxicam and caffeine as internal standard were dissolved in deuterated chloroform and then analyzed by ~1H-NMR. The delay time and number of scans were set as 12 s and 32,respectively. The peak of δ 2. 696 of piroxicam and δ 4. 006 of caffeine were selected as quantitative peak and internal standard peak,respectively. In the mass ratio range of 0. 25 ~ 6. 0,a good linear relationship was established with correlative coefficient( r~2) of 0. 9993 for piroxicam. The average recovery and relative standard deviation for piroxicam tablets were 97. 7% ~101. 0% and 0. 42% ~ 1. 2%,respectively. The content of piroxicam in tablets was in consistence with the labeled amount. The results showed that the q NMR method was reliable and could be applied to the measurement of piroxicam in sustained tablets.
引文
[1]Nationl Pharmacopoeia Committee.The Pharmacopoeia of the People's Republic of China(Part II,2015 Ed.).Beijing:China Medical Science Press国家药典委员会.中华人民共和国药典.二部.北京:中国医药科技出版社,2015
[2]Calvo A M,Prado M T O,Dionisio T J,et al.Original Res Pharmacol,2016,30(1):e58
[3]Liu H H.Chin J Modern Appl Pharm,2015,3(9):1125刘洪海.中国现代应用药学,2015,3(9):1125
[4]Zhang J M,Fu S W,Zhao J,et al.Chin J Anal Lab,2012,31(6):120张军民,傅思武,赵晋,等.分析试验室,2012,31(6):120
[5]Monakhova Y B,Kohl-Himmelseher M,Kuballa T,et al.J Pharm Biomed Anal,2014,100:381
[6]Sun L L,Zhang F F,Shen W B,et al.J Instrum Anal,2016,35(9):1157孙林林,张芬芬,沈文斌,等.分析测试学报,2016,35(9):1157
[7]Wu X F,Zhang Q,Ma L Y,et al.Chin J Pharm Anal,2017,37(1):181吴先福,张琪,马玲云,等.药物分析杂志,2017,37(1):181
[8]Liu M K,Guo S Q,Yu S,et al.Chin J Anal Lab,2015,34(11):1343刘明珂,郭胜强,禹珊,等.分析试验室,2015,34(11):1343
[9]Yu S,Guo Q S,Wang H L,et al.Chin J Anal Chem,2015,43(1):69禹珊,郭胜强,王会琳,等.分析化学,2015,43(1):69
[10]Li Xi D,Zhang W,Wang W H,et al.Chin J Anal Lab,2016,35(2):240李锡东,张伟,王卫华,等.分析试验室,2016,35(2):240
[11]Li Q Q,Zhu D,Pang X M,et al.C Chin J Anal Lab,2016,35(2):125李强强,朱丹,逄秀梅,等.分析试验室,2016,35(2):125
[2]Calvo A M,Prado M T O,Dionisio T J,et al.Original Res Pharmacol,2016,30(1):e58
[3]Liu H H.Chin J Modern Appl Pharm,2015,3(9):1125刘洪海.中国现代应用药学,2015,3(9):1125
[4]Zhang J M,Fu S W,Zhao J,et al.Chin J Anal Lab,2012,31(6):120张军民,傅思武,赵晋,等.分析试验室,2012,31(6):120
[5]Monakhova Y B,Kohl-Himmelseher M,Kuballa T,et al.J Pharm Biomed Anal,2014,100:381
[6]Sun L L,Zhang F F,Shen W B,et al.J Instrum Anal,2016,35(9):1157孙林林,张芬芬,沈文斌,等.分析测试学报,2016,35(9):1157
[7]Wu X F,Zhang Q,Ma L Y,et al.Chin J Pharm Anal,2017,37(1):181吴先福,张琪,马玲云,等.药物分析杂志,2017,37(1):181
[8]Liu M K,Guo S Q,Yu S,et al.Chin J Anal Lab,2015,34(11):1343刘明珂,郭胜强,禹珊,等.分析试验室,2015,34(11):1343
[9]Yu S,Guo Q S,Wang H L,et al.Chin J Anal Chem,2015,43(1):69禹珊,郭胜强,王会琳,等.分析化学,2015,43(1):69
[10]Li Xi D,Zhang W,Wang W H,et al.Chin J Anal Lab,2016,35(2):240李锡东,张伟,王卫华,等.分析试验室,2016,35(2):240
[11]Li Q Q,Zhu D,Pang X M,et al.C Chin J Anal Lab,2016,35(2):125李强强,朱丹,逄秀梅,等.分析试验室,2016,35(2):125