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Article(id=1200147947305398644, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1200147945191469403, articleNumber=1001-2494(2024)12-1151-05, orderNo=null, doi=10.11669/cpj.2024.12.011, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1702224000000, receivedDateStr=2023-12-11, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1764067168308, onlineDateStr=2025-11-25, pubDate=1718985600000, pubDateStr=2024-06-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1764067168308, onlineIssueDateStr=2025-11-25, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1764067168308, creator=13701087609, updateTime=1764067168308, updator=13701087609, issue=Issue{id=1200147945191469403, tenantId=1146029695717560320, journalId=1190317699101192196, year='2024', volume='59', issue='12', pageStart='1065', pageEnd='1170', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1764067167804, creator=13701087609, updateTime=1764067403507, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1200148933856035173, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1200147945191469403, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1200148933856035174, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1200147945191469403, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1151, endPage=1155, ext={EN=ArticleExt(id=1200147947519308159, articleId=1200147947305398644, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Determination of Reference Standards of Four Moxifloxacin Hydrochloride Impurities by Quantitative Proton Nuclear Magnetic Resonance, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To establish a quantitative proton nuclear magnetic resonance (qHNMR) method for determination of the reference standards of moxifloxacin hydrochloride impurities A, B, C and D. METHODS Proton nuclear magnetic resonance (1H-NMR) spectra of four reference standards of impurities were obtained in dimethylsulfoxide-d6 (DMSO-d6) or chloroform-d (CDCl3) using a nuclear magnetic resonance spectrometer. The internal standard was 1,3,5-trimethoxybenzene. All 1H-NMR spectra for quantitative analysis were measured with noesyigld1d pulse sequence using the following experimental parameters: 32 number of scans (NS), relaxation delay time (D1) of 30 s, 25 ℃ testing temperature. RESULTS The quantitative peak signals of four moxifloxacin hydrochloride impurities and 1, 3, 5-trimethoxybenzene were well separated on 1H-NMR spectra, and the linear relationship was good within the linear range (r2>0.999 4). The injection precision and repeatability of the method were good. The contents of four reference standards of impurities determined by qHNMR method were basically consistent with those determined by mass balance method. CONCLUSION The established qHNMR method is accurate, reliable, simple, fast, which provides a new way for content determination of these impurities and can also be used as a mutual verification method for the calibration results of these reference substance by the mass balance method.

, correspAuthors=Yong LU, Xianfu WU, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Yu HE, Yajun ZHANG, Jingxin XIE, Qing WANG, Changjun SHAO, Huimin SUN, Yong LU, Xianfu WU), CN=ArticleExt(id=1200147948228145563, articleId=1200147947305398644, tenantId=1146029695717560320, journalId=1190317699101192196, language=CN, title=定量核磁共振氢谱法测定4种盐酸莫西沙星杂质对照品的含量, columnId=1190352405612040510, journalTitle=中国药学杂志, columnName=论著, runingTitle=null, highlight=null, articleAbstract=

目的 建立测定4种盐酸莫西沙星杂质A、B、C、D对照品含量的定量核磁共振氢谱法 (quantitative proton nuclear magnetic resonance,qHNMR)。方法 采用核磁共振波谱仪采集4种盐酸莫西沙星杂质对照品的一维定量氢谱(1H-NMR),以1,3,5-三甲氧基苯作为内标物,氘代二甲亚砜(DMSO-d6)或氘代氯仿(CDCl3)作为溶剂,脉冲程序为noesyigld1d,扫描次数(NS)为32次,弛豫延迟时间(D1)为30 s,测试温度为25 ℃,对4种盐酸莫西沙星杂质对照品进行定量研究。结果 4种盐酸莫西沙星杂质对照品定量峰和1,3,5-三甲氧基苯定量峰信号在核磁共振氢谱上分离度良好,在线性范围内线性关系良好(r2>0.999 4),进样精密度和重复性良好。qHNMR法测定含量结果与质量平衡法测定含量结果基本一致。结论 建立的qHNMR法准确可靠、简便快速,为该类杂质含量测定提供了新的方法,也可作为该类化学对照品采用质量平衡法定值结果的验证方法。

, correspAuthors=路勇, 吴先富, authorNote=null, correspAuthorsNote=
*吴先富,男,博士,研究员 研究方向:药品质量控制及标准物质研究 Tel:(010)53852026;
路勇,男,博士,教授 研究方向:食品化妆品监管科学和标准物质研究 Tel:(010)53851515
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何雨,女,硕士研究生 研究方向:药物分析

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何雨,女,硕士研究生 研究方向:药物分析

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何雨,女,硕士研究生 研究方向:药物分析

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Chin Pharm J(中国药学杂志), 2023, 58(8): 725-729., articleTitle=Qualitative and quantitative analysis of residual solvent ethanol in three low molecular weight heparins by proton nuclear magnetic resonance, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1200147948488192427, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, xref=null, ext=[AuthorCompanyExt(id=1200147948496581036, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, companyId=1200147948488192427, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=National Institutes for Food and Drug Control, Beijing 102629, China), AuthorCompanyExt(id=1200147948504969645, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, companyId=1200147948488192427, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中国食品药品检定研究院, 北京 102629)])], figs=[ArticleFig(id=1200147951931716221, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=EN, label=Fig.1, caption=Chemical structures of moxifloxacin hydrochloride impurities A-D, figureFileSmall=k3Hh7opSYEvMkkLipEwzhg==, figureFileBig=/DEsqWxX5gfpqDus4YnAjw==, tableContent=null), ArticleFig(id=1200147952036573824, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=CN, label=图1, caption=盐酸莫西沙星杂质A~D的化学结构, figureFileSmall=k3Hh7opSYEvMkkLipEwzhg==, figureFileBig=/DEsqWxX5gfpqDus4YnAjw==, tableContent=null), ArticleFig(id=1200147952275649160, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=EN, label=Fig.2, caption=1H-NMR spectra of moxifloxacin hydrochloride impurities A-D, figureFileSmall=veDadiF+RIUcKnnzDxnX0g==, figureFileBig=FwMte5NvQrYFYjhl7LtZZw==, tableContent=null), ArticleFig(id=1200147952397283980, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=CN, label=图2, caption=盐酸莫西沙星杂质A~D的1H-NMR谱图, figureFileSmall=veDadiF+RIUcKnnzDxnX0g==, figureFileBig=FwMte5NvQrYFYjhl7LtZZw==, tableContent=null), ArticleFig(id=1200147952523113107, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=EN, label=Tab.1, caption=

T1 of moxifloxacin hydrochloride impurities A-D and the internal standard

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Impurity/internal standard δ T1/s
A 7.78(d,1H) 3.01
B 7.48(s,1H) 1.92
C 7.78(d,1H) 3.52
D 7.42(s,1H) 1.78
1,3,5-Trimethoxybenzene 6.10(s,3H) 2.99/4.22
), ArticleFig(id=1200147952615387799, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=CN, label=表1, caption=

盐酸莫西沙星杂质A~D以及内标物的继承弛豫时间(T1)

, figureFileSmall=null, figureFileBig=null, tableContent=
Impurity/internal standard δ T1/s
A 7.78(d,1H) 3.01
B 7.48(s,1H) 1.92
C 7.78(d,1H) 3.52
D 7.42(s,1H) 1.78
1,3,5-Trimethoxybenzene 6.10(s,3H) 2.99/4.22
), ArticleFig(id=1200147952732828314, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=EN, label=Tab.2, caption=

Regression equations and linear ranges of moxifloxacin hydrochloride impurities A-D

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Impurity Regression equation r2 Linear range
A Y=0.123 9X+0.008 6 0.999 6 1.11-12.16
B Y=0.104 3X+0.007 6 0.999 6 1.10-12.10
C Y=0.137 8X+0.006 6 0.999 4 1.29-14.22
D Y=0.135 4X+0.003 4 1.000 0 1.11-12.20
), ArticleFig(id=1200147952833491613, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=CN, label=表2, caption=

盐酸莫西沙星杂质A~D的回归方程与线性范围

, figureFileSmall=null, figureFileBig=null, tableContent=
Impurity Regression equation r2 Linear range
A Y=0.123 9X+0.008 6 0.999 6 1.11-12.16
B Y=0.104 3X+0.007 6 0.999 6 1.10-12.10
C Y=0.137 8X+0.006 6 0.999 4 1.29-14.22
D Y=0.135 4X+0.003 4 1.000 0 1.11-12.20
), ArticleFig(id=1200147952921572002, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=EN, label=Tab.3, caption=

Contents of moxifloxacin hydrochloride impurities A-D

, figureFileSmall=null, figureFileBig=null, tableContent=
Impurity Content/% Average
/%		 RSD
/%
1 2 3 4 5 6
A 98.36 97.49 97.73 96.37 99.01 97.55 97.75 0.91
B 88.24 87.40 87.32 87.16 88.26 87.78 87.69 0.54
C 101.23 99.55 100.81 99.87 101.07 100.31 100.47 0.67
D 97.58 98.58 98.29 98.38 97.89 98.66 98.23 0.43
), ArticleFig(id=1200147953018040995, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=CN, label=表3, caption=

盐酸莫西沙星杂质A~D含量测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
Impurity Content/% Average
/%		 RSD
/%
1 2 3 4 5 6
A 98.36 97.49 97.73 96.37 99.01 97.55 97.75 0.91
B 88.24 87.40 87.32 87.16 88.26 87.78 87.69 0.54
C 101.23 99.55 100.81 99.87 101.07 100.31 100.47 0.67
D 97.58 98.58 98.29 98.38 97.89 98.66 98.23 0.43
), ArticleFig(id=1200147953131287207, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=EN, label=Tab.4, caption=

Determination results of qHNMR and mass balance method

, figureFileSmall=null, figureFileBig=null, tableContent=
Impurity Content/%
qHNMR Mass balance method
A 97.75 98.24
B 87.69 88.82
C 100.47 99.60
D 98.23 98.89
), ArticleFig(id=1200147953257116334, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1200147947305398644, language=CN, label=表4, caption=

定量核磁共振氢谱法(qHNMR)与质量平衡法含量测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
Impurity Content/%
qHNMR Mass balance method
A 97.75 98.24
B 87.69 88.82
C 100.47 99.60
D 98.23 98.89
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定量核磁共振氢谱法测定4种盐酸莫西沙星杂质对照品的含量
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何雨 , 张雅军 , 谢晶鑫 , 王青 , 邵长军 , 孙会敏 , 路勇 * , 吴先富 *
中国药学杂志 | 论著 2024,59(12): 1151-1155
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中国药学杂志 | 论著 2024, 59(12): 1151-1155
定量核磁共振氢谱法测定4种盐酸莫西沙星杂质对照品的含量
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何雨, 张雅军, 谢晶鑫, 王青, 邵长军, 孙会敏, 路勇*, 吴先富*
作者信息
  • 中国食品药品检定研究院, 北京 102629

    • 何雨,女,硕士研究生 研究方向:药物分析

通讯作者:

*吴先富,男,博士,研究员 研究方向:药品质量控制及标准物质研究 Tel:(010)53852026;
路勇,男,博士,教授 研究方向:食品化妆品监管科学和标准物质研究 Tel:(010)53851515
Determination of Reference Standards of Four Moxifloxacin Hydrochloride Impurities by Quantitative Proton Nuclear Magnetic Resonance
Yu HE, Yajun ZHANG, Jingxin XIE, Qing WANG, Changjun SHAO, Huimin SUN, Yong LU*, Xianfu WU*
Affiliations
  • National Institutes for Food and Drug Control, Beijing 102629, China
出版时间: 2024-06-22 doi: 10.11669/cpj.2024.12.011
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摘要
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目的 建立测定4种盐酸莫西沙星杂质A、B、C、D对照品含量的定量核磁共振氢谱法 (quantitative proton nuclear magnetic resonance,qHNMR)。方法 采用核磁共振波谱仪采集4种盐酸莫西沙星杂质对照品的一维定量氢谱(1H-NMR),以1,3,5-三甲氧基苯作为内标物,氘代二甲亚砜(DMSO-d6)或氘代氯仿(CDCl3)作为溶剂,脉冲程序为noesyigld1d,扫描次数(NS)为32次,弛豫延迟时间(D1)为30 s,测试温度为25 ℃,对4种盐酸莫西沙星杂质对照品进行定量研究。结果 4种盐酸莫西沙星杂质对照品定量峰和1,3,5-三甲氧基苯定量峰信号在核磁共振氢谱上分离度良好,在线性范围内线性关系良好(r2>0.999 4),进样精密度和重复性良好。qHNMR法测定含量结果与质量平衡法测定含量结果基本一致。结论 建立的qHNMR法准确可靠、简便快速,为该类杂质含量测定提供了新的方法,也可作为该类化学对照品采用质量平衡法定值结果的验证方法。

定量核磁共振氢谱法  /  盐酸莫西沙星杂质  /  对照品  /  定值  /  含量测定

OBJECTIVE To establish a quantitative proton nuclear magnetic resonance (qHNMR) method for determination of the reference standards of moxifloxacin hydrochloride impurities A, B, C and D. METHODS Proton nuclear magnetic resonance (1H-NMR) spectra of four reference standards of impurities were obtained in dimethylsulfoxide-d6 (DMSO-d6) or chloroform-d (CDCl3) using a nuclear magnetic resonance spectrometer. The internal standard was 1,3,5-trimethoxybenzene. All 1H-NMR spectra for quantitative analysis were measured with noesyigld1d pulse sequence using the following experimental parameters: 32 number of scans (NS), relaxation delay time (D1) of 30 s, 25 ℃ testing temperature. RESULTS The quantitative peak signals of four moxifloxacin hydrochloride impurities and 1, 3, 5-trimethoxybenzene were well separated on 1H-NMR spectra, and the linear relationship was good within the linear range (r2>0.999 4). The injection precision and repeatability of the method were good. The contents of four reference standards of impurities determined by qHNMR method were basically consistent with those determined by mass balance method. CONCLUSION The established qHNMR method is accurate, reliable, simple, fast, which provides a new way for content determination of these impurities and can also be used as a mutual verification method for the calibration results of these reference substance by the mass balance method.

quantitative proton nuclear magnetic resonance  /  moxifloxacin hydrochloride impurity  /  reference standard  /  characterization  /  content determination
何雨, 张雅军, 谢晶鑫, 王青, 邵长军, 孙会敏, 路勇, 吴先富. 定量核磁共振氢谱法测定4种盐酸莫西沙星杂质对照品的含量. 中国药学杂志, 2024 , 59 (12) : 1151 -1155 . DOI: 10.11669/cpj.2024.12.011
Yu HE, Yajun ZHANG, Jingxin XIE, Qing WANG, Changjun SHAO, Huimin SUN, Yong LU, Xianfu WU. Determination of Reference Standards of Four Moxifloxacin Hydrochloride Impurities by Quantitative Proton Nuclear Magnetic Resonance[J]. Chinese Pharmaceutical Journal, 2024 , 59 (12) : 1151 -1155 . DOI: 10.11669/cpj.2024.12.011
正文
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盐酸莫西沙星(moxifloxacin hydrochloride)为第四代新型氟喹诺酮类合成抗菌药物,对革兰阴性菌和部分革兰阳性菌具有抗菌活性[1-2],不良反应小,主要用于社区获得性肺炎[3]、细菌性眼部感染[4]、下呼吸道感染[5]、泌尿生殖系统感染和急慢性鼻窦炎[6]等疾病的治疗。盐酸莫西沙星杂质A(1-环丙基-6,8-二氟-1,4-二氢-7-[(4aS,7aS)-八氢-6H-吡咯并[4-b]吡啶-6-基]-4-氧代-3-喹啉羧酸)、盐酸莫西沙星杂质B(1-环丙基-6,8-二甲氧基-1,4-二氢-7-[(4aS,7aS)-八氢-6-吡咯并[4-b]吡啶-6-基]-4-氧代-3-喹啉羧酸)、盐酸莫西沙星杂质C(1-环丙基-8-乙氧基-6-氟-1,4-二氢-7-[(4aS,7aS)-八氢-6-吡咯并[4-b]吡啶-6-基]-4-氧代-3-喹啉羧酸)和盐酸莫西沙星杂质D(1-环丙基-8-氟-6-甲氧基-1,4-二氢-7-[(4aS,7aS)-八氢-6-吡咯并[4-b]吡啶-6-基]-4-氧代-3-喹啉羧酸)(结构见图1)均在《美国药典》[7]、《欧洲药典》[8]和我国注册标准中盐酸莫西沙星品种项下收载[9-12]。目前,对上述杂质的测定,通常采用高效液相色谱法[13]。对其化学对照品的定值方法,通常采用质量平衡法(mass balance method),即标准物质的杂质、水分、残留溶剂、无机杂质、主成分成盐离子与活性成分含量的和为100%[14],但是该方法的准确性可能会受到某些因素的影响,例如色谱峰的分离度、色谱峰的响应因子等[15]。定量核磁共振氢谱技术(quantitative proton nuclear magnetic resonance, qHNMR)现已广泛应用在新药研发、药物质量控制和标准物质定值等领域,该方法为无歧视检测方法,具有适用范围广、无须标准物质、样品制备简便和检测速度快等优势[16-17]。
本实验建立了4种盐酸莫西沙星杂质对照品的qHNMR,该方法准确可靠、简便快速,为该类杂质含量的测定提供了新的方法,也可作为该类化学对照品采用质量平衡法定值结果的验证方法。
1 仪器与试药
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1.1 仪器
Bruker Ascend 600型核磁共振波谱仪(德国Bruker公司);MSA125P-1CE-DI电子天平(美国Sartorius公司)。
1.2 试药
1,3,5-三甲氧基苯(批号:510137-201601,含量:99.9%)、盐酸莫西沙星杂质A(批号:510074-202102)、盐酸莫西沙星杂质B(批号:510075-202302)、盐酸莫西沙星杂质C(批号:510076-202102)和盐酸莫西沙星杂质D(批号:510190-202102)(中国食品药品检定研究院);氘代二甲亚砜(DMSO-d6,批号:PR-32855/07191DM1,美国剑桥同位素实验室);氘代氯仿(CDCl3,批号:225789-100G,美国Sigma-Aldrich公司)。
2 方法
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2.1 供试品溶液制备
取4种盐酸莫西沙星杂质A,B,C,D对照品各10 mg,精密称定,加入3 mL 氘代试剂使其完全溶解(盐酸莫西沙星杂质C以CDCl3为溶剂,其余杂质以DMSO-d6为溶剂)。取1,3,5-三甲氧基苯10 mg,精密称定,加入10 mL DMSO-d6(CDCl3)使其完全溶解。取样品溶液1 mL,精密加入内标溶液0.5 mL,摇匀,即得供试品溶液,取适量溶液转移至5 mm核磁管中备用。
2.2 核磁仪器参数设置
采用90°脉冲,脉冲程序为noesyigld1d,谱宽(SWH)设置为11 904.762 Hz,空扫次数(DS)为4次,扫描次数(NS)为32次,采样时间(AQ)为2.75 s,采样点数(TD)为6.553 6×107,接收器增益(RG)为32,弛豫延迟时间(D1)为30 s。
2.3 数据处理qNMR计算
采用Bruker TopSpin 4.1.3软件进行数据处理,将采集到的一维氢谱进行傅里叶变换,然后对图谱进行基线校正和相位校正。对内标定量峰与样品定量峰进行积分,每个峰积分次数不少于5次,取峰面积的平均值,根据公式1[18]计算4种盐酸莫西沙星杂质对照品的含量结果。
含量(%)= A s p l A s t d× n s t d n s p l× M s p l M s t d× W s p l W s t d
其中,Aspl,Astd分别为样品与内标物定量峰的积分面积;nstd,nspl分别为样品与内标物定量峰所包含的质子数;Mspl,Mstd分别为样品与内标物的相对分子质量;Wspl,Wstd分别为样品与内标物称样量。
3 结果与讨论
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3.1 溶剂与内标物的选择
选择的溶剂应对样品和内标物均有较好溶解度,不与二者发生反应,且在1H-NMR中溶剂的定量峰信号对样品及内标物的定量峰信号不产生干扰。由于盐酸莫西沙星杂质A、B和D在DMSO-d6中易溶。盐酸莫西沙星杂质C在CDCl3中易溶。因此,前3种杂质选用DMSO-d6作为溶剂,后一种杂质选择CDCl3作为溶剂。选择的内标物应该具有稳定的化学性质、不与待测物发生反应、能与样品溶解于同一种氘代试剂中,且在核磁共振氢谱中其定量峰信号与样品定量峰信号不重叠等。按照上述要求,选择1,3,5-三甲氧基苯作为内标物。
3.2 样品定量峰的选择
选择的样品定量峰应与相邻峰分离良好,与内标物定量峰互不干扰。在1H-NMR谱图(图2)中,盐酸莫西沙星杂质A、B、C和D分别选择苯环质子(δ 7.78,7.48,7.78,7.42)[19]峰信号作为定量峰。内标物1,3,5-三甲氧基苯选择δ 6.10处峰信号作为定量峰。
3.3 仪器参数的选择
弛豫延迟时间(D1)是影响NMR信号积分值的重要因素,D1与纵向弛豫时间(T1)直接相关。采用反转恢复实验[20],测得盐酸莫西沙星杂质C和内标物在CDCl3中的T1值为3.52和4.22 s(表1),其余3种盐酸莫西沙星杂质和内标物在DMSO-d6中的T1值为1.78~3.01 s(表1),qHNMR实验中D1的设定值通常不小于5倍的T1值[21],因此,最终D1值设定为30 s。
3.4 方法学考察
3.4.1 线性关系考察
取样品与内标物按照“2.1”项下方法制备样品溶液与内标溶液。分别吸取不同体积的样品溶液和内标溶液,混合,摇匀,得到6份不同浓度供试品溶液,按“2.2”项条件测定。以样品与内标物的质量比值为横坐标,样品定量峰与内标定量峰面积比值为纵坐标,绘制标准曲线,得到回归方程(表2)。
3.4.2 仪器精密度试验
取样品,按照“2.1”项下方法制备供试品溶液,按“2.2”项下条件连续测定6次,计算盐酸莫西沙星杂质A、B、C和D的样品定量峰与内标定量峰面积比值的相对标准偏差(RSD)(n=6)分别为0.08%、0.31%、0.16%和0.68%。
3.4.3 重复性试验
取样品,按照“2.1”项下方法平行制备6份供试品溶液,按“2.2”项下条件测定,盐酸莫西沙星杂质A、B、C和D的样品含量测定结果见表3。结果表明,重复性良好。
3.4.4 稳定性试验
取样品,按照“2.1”项下方法制备供试品溶液,按“2.2”项下条件于0、4、8、12、24和48 h进行测定,盐酸莫西沙星杂质A、B、C和D样品定量峰与内标峰面积比值的RSD分别为0.27%、0.80%、0.41%和0.40%,表明样品溶液在48 h内基本保持稳定。
3.4.5 检测限和定量限
取样品,按照“2.1”项下方法制备供试品溶液,测得的信噪比(S/N)分别为7 950.18、1 023.82、5 935.65、47 588.01,为以定量峰的S/N=3计,盐酸莫西沙星杂质A、B、C和D的检测限分别为0.83,6.51,1.12,0.14 μg·mL-1。为以定量峰的S/N=250计[22],盐酸莫西沙星杂质A、B、C和D的定量限分别为69.88,542.63,93.60,11.67 μg·mL-1。
3.5 qHNMR法与质量平衡法结果比较
化学对照品定值通常采用质量平衡法(公式2),根据该方法测定盐酸莫西沙星杂质A、B、C和D,含量测定结果见表4。结果表明,qHNMR法测定的含量结果与质量平衡法测定结果基本一致。
含量(%)=(100%-干燥失重值%-炽灼残渣值%)×HPLC纯度
4 结论
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建立了测定盐酸莫西沙星杂质对照品A、B、C和D含量的qHNMR法,该方法操作简便、检测速度快、测定结果专属性强且检测过程中不破坏样品,为该类杂质含量测定提供了新方法。该方法测定含量结果与质量平衡法测定含量结果基本一致,说明该方法的含量测定结果也可作为该类对照品质量平衡法的测定结果的验证方法,确保该类化学对照品定值准确。
文献
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2024年第59卷第12期
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doi: 10.11669/cpj.2024.12.011
  • 接收时间：2023-12-11
  • 首发时间：2025-11-25
  • 出版时间：2024-06-22
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  • 收稿日期：2023-12-11
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    中国食品药品检定研究院, 北京 102629

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*吴先富,男,博士,研究员 研究方向:药品质量控制及标准物质研究 Tel:(010)53852026;
路勇,男,博士,教授 研究方向:食品化妆品监管科学和标准物质研究 Tel:(010)53851515
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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