硫酸异帕米星标准物质的研制
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摘要
目的:为满足国内硫酸异帕米星质量控制需要,标定了硫酸异帕米星对照品的含量。方法:采用质谱、核磁共振等技术对硫酸异帕米星中异帕米星的结构进行确证,并首次对该化合物的核磁信号进行了准确归属。采用质量平衡法确定了硫酸异帕米星中异帕米星的含量并进一步利用核磁定量法(QNMR)对上述结果进行佐证。结果:本批硫酸异帕米星对照品的含量按异帕米星(C22H43N5O12)计为70. 9%。结论:建立了首批硫酸异帕米星标准物质。
Objective: In order to assure the quality of isepamicin sulfate products in Chinese market,the content of new reference standard for isepamicin sulfate will be determined in this study. Methods: The structure of isepamicin in isepamicin sulfate was identified by LC-MS and NMR and the nuclear magnetic signal of the compound was accurately classified for the first time. The content of isepamicin was determined by mass balance method and the above result was further proved by the quantitative nuclear magnetic resonance( QNMR) method.Results: The content of isepamicin sulfate in this batch is 70. 9% according to isepamicin( C22 H43 N5 O12).Conclusion: The first batch of national standard substances of isepamicin sulfate was successfully developed.
Objective: In order to assure the quality of isepamicin sulfate products in Chinese market,the content of new reference standard for isepamicin sulfate will be determined in this study. Methods: The structure of isepamicin in isepamicin sulfate was identified by LC-MS and NMR and the nuclear magnetic signal of the compound was accurately classified for the first time. The content of isepamicin was determined by mass balance method and the above result was further proved by the quantitative nuclear magnetic resonance( QNMR) method.Results: The content of isepamicin sulfate in this batch is 70. 9% according to isepamicin( C22 H43 N5 O12).Conclusion: The first batch of national standard substances of isepamicin sulfate was successfully developed.
引文
[1]王建,阮丹,王知坚. HPLC-ELSD分析硫酸异帕米星及其注射液[J].中国现代应用药学,2013,30(4):411-416.
[2]赵敬丹,王曦,秦峰,等.柱后衍生化-HPLC法测定硫酸异帕米星注射液的含量和有关物质[J].中国抗生素杂志,2017,42(5):363-368.
[3]王明娟,成双红,张斗胜,等. HPLC-ELSD法测定异帕米星含量[J].中国抗生素杂志,2003,28(1):20-22.
[4] VOGEL R,DEFILLIPO K,REIF V. Determination of isepamicin sulfate and related compounds by high performance liquid chromatography using evaporative light scattering detection[J]. J Pharm Biomed Anal,2001,24(3):405-412.
[5] TOD M,PADOIN C,PETITJEAN O. Clinical pharmacokinetics and pharmacodynamics of isepamicin[J]. Clin Pharmacokinet,2000,38(3):205-223.
[6]国家药典委员会.中华人民共和国药典[S]. 2015年版.第二部.北京:中国医药科技出版社,2015:1328-1330.
[7] Japanese Pharmacopeia. The Society of Japanese Pharmacopeia[S] 2016 pp. XⅦ. Japan:Japanese Pharmacopeia,2016:1093-1094.
[8]王建,王巧群,孙进,等.硫酸异帕米星中有关物质的分离、鉴定和抗菌活性研究[J].中国药学杂志,2007,42(2):150-153.
[9]冯艳春,刘书妤,胡昌勤.比阿培南标准物质的研制[J].中国抗生素杂志,2010,35(9):679-683.
[10]周晓力,陈华,南楠.1H NMR定量测D3-吗啡对照品的含量[J].药物分析杂志,2015,35(5):906-909.
[11] BHARTI SK,ROY R. Quantitative1H NMR spectroscopy[J].Trends Anal Chem,2012,35:5-26.
[12] MANIARA G,RAJAMOORTHI K,RAJAN S,et al. Methodperformance and validation for quantitative analysis by1H and31P NMR spectroscopy. Application to analytical standards and agricultural chemicals[J]. Anal Chem,1998,70(23):4921-4928.
[13]张永权,冯艳春,李进,等.酮康唑相关杂质国家标准物质的研制[J].药物分析杂志,2015,35(3):532-542.
[14]吴迪,陈华,王腾,等.19F核磁共振定量法测定吉非替尼的含量[J].中国新药杂志,2017,26(19):2343-2346.
[15]李煜,张淼,吴冬燕,等.13C核磁共振技术测定鱼肝油中ω-3脂肪酸α(1,3)-酰基和β(2)-酰基的位次分布[J].中国现代应用药学,2017,34(11):1582-1584.
[2]赵敬丹,王曦,秦峰,等.柱后衍生化-HPLC法测定硫酸异帕米星注射液的含量和有关物质[J].中国抗生素杂志,2017,42(5):363-368.
[3]王明娟,成双红,张斗胜,等. HPLC-ELSD法测定异帕米星含量[J].中国抗生素杂志,2003,28(1):20-22.
[4] VOGEL R,DEFILLIPO K,REIF V. Determination of isepamicin sulfate and related compounds by high performance liquid chromatography using evaporative light scattering detection[J]. J Pharm Biomed Anal,2001,24(3):405-412.
[5] TOD M,PADOIN C,PETITJEAN O. Clinical pharmacokinetics and pharmacodynamics of isepamicin[J]. Clin Pharmacokinet,2000,38(3):205-223.
[6]国家药典委员会.中华人民共和国药典[S]. 2015年版.第二部.北京:中国医药科技出版社,2015:1328-1330.
[7] Japanese Pharmacopeia. The Society of Japanese Pharmacopeia[S] 2016 pp. XⅦ. Japan:Japanese Pharmacopeia,2016:1093-1094.
[8]王建,王巧群,孙进,等.硫酸异帕米星中有关物质的分离、鉴定和抗菌活性研究[J].中国药学杂志,2007,42(2):150-153.
[9]冯艳春,刘书妤,胡昌勤.比阿培南标准物质的研制[J].中国抗生素杂志,2010,35(9):679-683.
[10]周晓力,陈华,南楠.1H NMR定量测D3-吗啡对照品的含量[J].药物分析杂志,2015,35(5):906-909.
[11] BHARTI SK,ROY R. Quantitative1H NMR spectroscopy[J].Trends Anal Chem,2012,35:5-26.
[12] MANIARA G,RAJAMOORTHI K,RAJAN S,et al. Methodperformance and validation for quantitative analysis by1H and31P NMR spectroscopy. Application to analytical standards and agricultural chemicals[J]. Anal Chem,1998,70(23):4921-4928.
[13]张永权,冯艳春,李进,等.酮康唑相关杂质国家标准物质的研制[J].药物分析杂志,2015,35(3):532-542.
[14]吴迪,陈华,王腾,等.19F核磁共振定量法测定吉非替尼的含量[J].中国新药杂志,2017,26(19):2343-2346.
[15]李煜,张淼,吴冬燕,等.13C核磁共振技术测定鱼肝油中ω-3脂肪酸α(1,3)-酰基和β(2)-酰基的位次分布[J].中国现代应用药学,2017,34(11):1582-1584.