Article(id=1236346592672936398, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1236346588398932061, articleNumber=null, orderNo=null, doi=null, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=null, revisedDateStr=null, acceptedDate=1669305600000, acceptedDateStr=2022-11-25, onlineDate=1772697597901, onlineDateStr=2026-03-05, pubDate=1685376000000, pubDateStr=2023-05-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772697597901, onlineIssueDateStr=2026-03-05, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772697597901, creator=13701087609, updateTime=1772697597901, updator=13701087609, issue=Issue{id=1236346588398932061, tenantId=1146029695717560320, journalId=1235980733773295621, year='2023', volume='32', issue='10', pageStart='969', pageEnd='1072', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1772697596882, creator=13701087609, updateTime=1772697715363, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1236347085411373506, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1236346588398932061, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1236347085411373507, tenantId=1146029695717560320, journalId=1235980733773295621, issueId=1236346588398932061, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1064, endPage=1072, ext={EN=ArticleExt(id=1236346592874263005, articleId=1236346592672936398, tenantId=1146029695717560320, journalId=1235980733773295621, language=EN, title=Screening and compatibility study of 20 elements in Shenlu Tablets by microwave digestion-ICP-MS, columnId=null, journalTitle=Chinese Journal of New Drugs, columnName=null, runingTitle=null, highlight=null, articleAbstract=
Objective:

To investigate the compatibility between Shenlu Tablets and drug packaging materials by screening and determination of 20 elements in Shenlu Tablets.

Methods:

For accelerated testing, the samples were stored at a temperature of 40 ℃ and a relative humidity of 90% for 0, 1, 2, and 3 months. Compatibility study was carried out by comparing the content of elements. At the same time, elemental determination was carried out on the corresponding raw and auxiliary materials of Shenlu Tablets to determine the source of the elements. Elements that were classified as 1, 2A, 2B (As,Cd,Pb,Hg,Co,V,Ni,Ag) were used as risk assessment elements using ICH Q3D. Risk elements in ginseng deer supplements were assessed according to "Chinese Pharmacopoeia" 2020 Edition Fourth General Chapter 9302 Harmful Traditional Chinese Medicine Guidelines.

Results:

The 20 elements showed a good linearty, with the correlation coefficient r of 0.997 3~0.999 9, the recovery rate of spiked sample of 92.7%~98.4%, and the recovery rate of drug packaging material of 82.1%~101.7%. The detection limits of all elements were within 0.000 17~0.17 μg·g-1. 19 elements except Hg were detected in Shenlu Tablets. Except for As, Ag, Sb, Hg, Bi, the other 15 elements were detected in the packaging materials used for the patch. Among the raw and auxiliary materials corresponding to Shenlu Tablets, the elements detected in the traditional Chinese medicinal materials are basically the same without obvious element aggregation. The compatibility results show that, compared with the results of the accelerated test in 3 months and in 0 months, six was no obvious migration of each element in the patch and the corresponding packaging material for the three batches of Shenlu Tablets. The maximum theoretical limit of 8 risk elements in Shenlu Tablets was compared with the average content of the accelerated test samples, and the average content of the samples was far less than the maximum theoretical limit L value.

Conclusion:

The microwave digestion-ICP-MS was used to determine 20 elements in Shenlu Tablets with high precision, repeatability and stability. There is no significant difference in the contribution of different Chinese herbal medicines to the elements in Shenlu supplement, and there does not exist single source. Combining the results of compatibility and risk analysis, the compatibility between the drug and the packaging material is good, and the risk of element intake is low. This study helps comprehensively evaluate the safety and compatibility of the drug, providing a reference for the quality control of similar drugs and the establishment of element intake risk assessment.

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目的:

通过对参鹿补片中20种元素的筛查测定,考察参鹿补片与药包材之间的相容性。

方法:

样品于温度40 ℃,相对湿度90%的环境中分别放置0,1,2,3个月进行加速实验,对加速后的药品与药包材采用微波消解-电感耦合等离子体质谱(ICP-MS)法测定其20种元素的含量,比较元素的含量变化进行相容性研究。同时对参鹿补片对应的原辅料进行元素测定,确定元素的来源。通过ICH Q3D确定分级为1,2A,2B的元素(As,Cd,Pb,Hg,Co,V,Ni,Ag)作为本实验风险评估的元素,结合《中华人民共和国药典》2020年版四部通则9302“中药有害残留物限量制定指导原则”对参鹿补片中的风险元素进行评估。

结果:

20种元素线性关系良好,相关系数(r)为0.997 3~0.999 9,药品加标回收率为92.7%~98.4%,药包材加标回收率为82.1%~101.7%,所有元素的检出限在0.000 17~0.17 μg·g-1之间;参鹿补片中检出除Hg元素外的19种元素。在补片所用包材中除As,Ag,Sb,Hg,Bi外,其余15种均有检出。在参鹿补片对应的原辅料中,中药材检出的元素种类基本相同,无明显元素聚集;相容性研究结果显示:加速实验3个月与0个月测定结果比较,6批参鹿补片和对应的包材中各元素未存在明显迁移。8种风险元素在参鹿补片中的最大理论限量与加速实验样品中的平均含量比较,样品中的平均含量均远小于最大理论限量L值。

结论:

采用微波消解-ICP-MS法测定参鹿补片中的20种元素,方法精密度、重复性、稳定性高。参鹿补片对应中药材对参鹿补片中元素的贡献无明显区别,不存在单一来源。结合相容性和风险分析结果,药品与包材之间的相容性良好,元素摄入风险低。该研究有助于综合评价该药的安全性、相容性,为同类品种药品的质量控制、元素摄入风险评估建立提供参考。

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朱碧君,女,学士,主任药师,主要从事药包材质量分析与相容性研究。E-mail:
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汪元亮,男,硕士,工程师,主要从事药包材质量分析与相容性研究。E-mail:

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采用微波消解-电感耦合等离子体质谱法对中药制剂参鹿补片中20种元素的筛查及相容性研究
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汪元亮 1 , 肖小武 1 , 朱碧君 1 , 黄武军 2 , 鄢章龙 2
中国新药杂志 | 实验研究 2023,32(10): 1064-1072
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中国新药杂志 | 实验研究 2023, 32(10): 1064-1072
采用微波消解-电感耦合等离子体质谱法对中药制剂参鹿补片中20种元素的筛查及相容性研究
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汪元亮1 , 肖小武1, 朱碧君1 , 黄武军2, 鄢章龙2
作者信息
  • 1江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029
  • 2江西药都仁和制药有限公司,樟树 331200
  • 汪元亮,男,硕士,工程师,主要从事药包材质量分析与相容性研究。E-mail:

通讯作者:

朱碧君,女,学士,主任药师,主要从事药包材质量分析与相容性研究。E-mail:
Screening and compatibility study of 20 elements in Shenlu Tablets by microwave digestion-ICP-MS
Yuan-liang WANG1 , Xiao-wu XIAO1, Bi-jun ZHU1 , Wu-jun HUANG2, Zhang-long YAN2
Affiliations
  • 1Jiangxi Institute for Drug Control, NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine, Jiangxi Province Engineering Research Center of Drug and Medical Device Quality, Nanchang 330029, China
  • 2Jiangxi Yaodu Renhe Pharmaceutial Co., Ltd., Zhangshu 331200, China
出版时间: 2023-05-30
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目的:

通过对参鹿补片中20种元素的筛查测定,考察参鹿补片与药包材之间的相容性。

方法:

样品于温度40 ℃,相对湿度90%的环境中分别放置0,1,2,3个月进行加速实验,对加速后的药品与药包材采用微波消解-电感耦合等离子体质谱(ICP-MS)法测定其20种元素的含量,比较元素的含量变化进行相容性研究。同时对参鹿补片对应的原辅料进行元素测定,确定元素的来源。通过ICH Q3D确定分级为1,2A,2B的元素(As,Cd,Pb,Hg,Co,V,Ni,Ag)作为本实验风险评估的元素,结合《中华人民共和国药典》2020年版四部通则9302“中药有害残留物限量制定指导原则”对参鹿补片中的风险元素进行评估。

结果:

20种元素线性关系良好,相关系数(r)为0.997 3~0.999 9,药品加标回收率为92.7%~98.4%,药包材加标回收率为82.1%~101.7%,所有元素的检出限在0.000 17~0.17 μg·g-1之间;参鹿补片中检出除Hg元素外的19种元素。在补片所用包材中除As,Ag,Sb,Hg,Bi外,其余15种均有检出。在参鹿补片对应的原辅料中,中药材检出的元素种类基本相同,无明显元素聚集;相容性研究结果显示:加速实验3个月与0个月测定结果比较,6批参鹿补片和对应的包材中各元素未存在明显迁移。8种风险元素在参鹿补片中的最大理论限量与加速实验样品中的平均含量比较,样品中的平均含量均远小于最大理论限量L值。

结论:

采用微波消解-ICP-MS法测定参鹿补片中的20种元素,方法精密度、重复性、稳定性高。参鹿补片对应中药材对参鹿补片中元素的贡献无明显区别,不存在单一来源。结合相容性和风险分析结果,药品与包材之间的相容性良好,元素摄入风险低。该研究有助于综合评价该药的安全性、相容性,为同类品种药品的质量控制、元素摄入风险评估建立提供参考。

参鹿补片  /  元素  /  电感耦合等离子体质谱法  /  微波消解  /  相容性
Objective:

To investigate the compatibility between Shenlu Tablets and drug packaging materials by screening and determination of 20 elements in Shenlu Tablets.

Methods:

For accelerated testing, the samples were stored at a temperature of 40 ℃ and a relative humidity of 90% for 0, 1, 2, and 3 months. Compatibility study was carried out by comparing the content of elements. At the same time, elemental determination was carried out on the corresponding raw and auxiliary materials of Shenlu Tablets to determine the source of the elements. Elements that were classified as 1, 2A, 2B (As,Cd,Pb,Hg,Co,V,Ni,Ag) were used as risk assessment elements using ICH Q3D. Risk elements in ginseng deer supplements were assessed according to "Chinese Pharmacopoeia" 2020 Edition Fourth General Chapter 9302 Harmful Traditional Chinese Medicine Guidelines.

Results:

The 20 elements showed a good linearty, with the correlation coefficient r of 0.997 3~0.999 9, the recovery rate of spiked sample of 92.7%~98.4%, and the recovery rate of drug packaging material of 82.1%~101.7%. The detection limits of all elements were within 0.000 17~0.17 μg·g-1. 19 elements except Hg were detected in Shenlu Tablets. Except for As, Ag, Sb, Hg, Bi, the other 15 elements were detected in the packaging materials used for the patch. Among the raw and auxiliary materials corresponding to Shenlu Tablets, the elements detected in the traditional Chinese medicinal materials are basically the same without obvious element aggregation. The compatibility results show that, compared with the results of the accelerated test in 3 months and in 0 months, six was no obvious migration of each element in the patch and the corresponding packaging material for the three batches of Shenlu Tablets. The maximum theoretical limit of 8 risk elements in Shenlu Tablets was compared with the average content of the accelerated test samples, and the average content of the samples was far less than the maximum theoretical limit L value.

Conclusion:

The microwave digestion-ICP-MS was used to determine 20 elements in Shenlu Tablets with high precision, repeatability and stability. There is no significant difference in the contribution of different Chinese herbal medicines to the elements in Shenlu supplement, and there does not exist single source. Combining the results of compatibility and risk analysis, the compatibility between the drug and the packaging material is good, and the risk of element intake is low. This study helps comprehensively evaluate the safety and compatibility of the drug, providing a reference for the quality control of similar drugs and the establishment of element intake risk assessment.

Shenlubu Tablets  /  elements  /  ICP-MS  /  microwave digestion  /  compatibility
汪元亮, 肖小武, 朱碧君, 黄武军, 鄢章龙. 采用微波消解-电感耦合等离子体质谱法对中药制剂参鹿补片中20种元素的筛查及相容性研究. 中国新药杂志, 2023 , 32 (10) : 1064 -1072 .
Yuan-liang WANG, Xiao-wu XIAO, Bi-jun ZHU, Wu-jun HUANG, Zhang-long YAN. Screening and compatibility study of 20 elements in Shenlu Tablets by microwave digestion-ICP-MS[J]. Chinese Journal of New Drugs, 2023 , 32 (10) : 1064 -1072 .
  • 江西省科技厅项目(20223BBG71001)
  • 江西省药品监督管理局科研项目(2021KY13)
2023年第32卷第10期
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  • 首发时间:2026-03-05
  • 出版时间:2023-05-30
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  • 录用日期:2022-11-25
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江西省科技厅项目(20223BBG71001)
江西省药品监督管理局科研项目(2021KY13)
作者信息
    1江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029
    2江西药都仁和制药有限公司,樟树 331200

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朱碧君,女,学士,主任药师,主要从事药包材质量分析与相容性研究。E-mail:
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

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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