基于气相色谱的六神系列制剂中人工麝香的特征图谱和含量测定

doi:10.3976/j.issn.1002-4026.2025021

Abstract

Abstract:

A scientific, unified, and reliable characteristic chromatograms and determine the content of artificial musk in the Liushen series of preparations was established using gas chromatography (GC) to accurately reflect its quality, providing an experimental basis for subsequent revisions of quality standards. The similarity of characteristic chromatograms from 39 batches of Liushen series preparations was analyzed using Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation Software(2012 version), with similarities all above 0.995. Liushen pills exhibited 5 characteristic peaks, while Liushen capsules showed 4, one of which was identified as muscone. The content of artificial musk in three types of preparations was determined, with muscone showing a good linear relationship within the range of 0.006 4~0.638 8 mg/mL(R=0.999). The average recovery rates(relative standard deviation) for pills, capsules, and gel agents were 102.3% (1.0%), 97.3% (1.5%), and 103.1% (1.6%) respectively. The established GC characteristic chromatograms and content determination method can comprehensively reflect the quality of artificial musk in LiuShen series preparations and can be used for quality control of artificial musk in these preparations.

Key words: Liushen series preparations, artificial musk, muscone, characteristic chromatograms, gas chromatography, content determination

CLC Number:

R284.2

GUO Lumei, WANG Yingchao, ZHANG Zhenkai, LIU Xingpeng, CHEN Feng. Characteristic chromatograms and content determination of artificial musk in Liushen series preparations based on gas chromatography[J].Shandong Science, 2025, 38(6): 42-51.

Figures/Tables 10

Fig.1

Fig.2

Fig.3

Fig.4

Fig.5

Table 1

Fig.6

Table 2

Table 3

Table 4

References 14

[1]	李文良. 六神丸的临床应用及实验研究进展[J]. 中成药, 1994, 16(1): 44-45.
[2]	韩珊珊, 刘寨东. 六神丸抗肿瘤作用研究进展[J]. 江苏中医药, 2022, 54(6): 79-82. DOI: 10.19844/j.cnki.1672-397X.2022.06.024.
[3]	李滢, 刘寨东. 基于毒攻疗法论六神丸外用治疗癌性溃疡[J]. 中医药学报, 2024, 52(2): 62-65. DOI: 10.19664/j.cnki.1002-2392.240034.
[4]	陈泽兴. 基于NLRP3炎症小体通路探讨六神丸抗甲型流感病毒所致炎症的机制研究[D]. 广州: 广州医科大学, 2023. DOI: 10.27043/d.cnki.ggzyc.2023.000725.
[5]	朱嘉亮, 郗昊, 冯磊, 等. 国家药品抽检检验机构实验室管理风险点分析及对策[J]. 医药导报, 2025, 44(1): 68-72. DOI: 10.3870/j.issn.1004-0781.2025.01.008.
[6]	朱嘉亮, 陈蕾, 王翀, 等. 基于问题导向的国家药品抽检计划设计方法探讨[J]. 医药导报, 2023, 42(3): 436-442. DOI: 10.3870/j.issn.1004-0781.2023.03.027.
[7]	王鑫, 李俊松, 狄留庆, 等. HPLC法测定六神丸中游离胆红素及总胆红素含量[J]. 现代中药研究与实践, 2020, 34(2): 60-64. DOI: 10.13728/j.1673-6427.2020.02.012.
[8]	李宗云, 刘莉, 何世学, 等. 一测多评法测定六神丸中5种蟾毒配基类成分含量[J]. 中国医院药学杂志, 2020, 40(2): 184-188. DOI: 10.13286/j.1001-5213.2020.02.11.
[9]	韩加伟, 曹慧敏, 燕珂, 等. 六神丸指纹图谱及其6种指标成分含量测定的研究[J]. 中国新药杂志, 2020, 29(3): 329-334. DOI: 10.3969/j.issn.1003-3734.2020.03.016.
[10]	龚晓丽, 王剑波, 罗霜, 等. 含有麝香中成药的质量研究现状[J]. 中国现代中药, 2023, 25(5): 1155-1162. DOI: 10.13313/j.issn.1673-4890.20220524002.
[11]	国家药典委员会. 中华人民共和国药典2020年版一部[S]. 北京: 中国医药科技出版社, 2020: 402-403.
[12]	久牧. 人工麝香研制及其产业化[J]. 中国食品药品监管, 2016(4): 62-65.
[13]	齐娜, 段文娟, 李雅婧, 等. 麝香酮药理作用的研究进展[J]. 世界科学技术-中医药现代化, 2020, 22(8): 3042-3047. DOI: 10.11842/wst.20181223004.
[14]	翟永松, 王大伟, 李鹏跃, 等. 九味防瘟散中麝香酮的含量测定及稳定性研究[J]. 中国实验方剂学杂志, 2013, 19(10): 128-130.

Metrics

Comments

Recommended 0

Open Access This article is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License (CC BY-NC 4.0), which permits third parties to freely share (i.e., copy and redistribute the material in any medium or format) and adapt (i.e., remix, transform, or build upon the material) the articles published in this journal, provided that appropriate credit is given, a link to the license is provided, and any changes made are indicated. The material may not be used for commercial purposes. For details of the CC BY-NC 4.0 license, please visit: https://creativecommons.org/licenses/by-nc/4.0

剂型	生产企业	样品编号	相似度	剂型	生产企业	样品编号	相似度
六神丸	A	LSW01	0.999	六神丸	A	LSW10	1.000
	A	LSW02	0.999		A	LSW11	1.000
	A	LSW03	0.997		B	LSW12	1.000
六神丸	A	LSW04	0.999	六神丸	B	LSW13	1.000
	A	LSW05	0.999		B	LSW14	1.000
	A	LSW06	1.000		B	LSW15	0.999
	A	LSW07	0.998		B	LSW16	1.000
	A	LSW08	0.999		B	LSW17	1.000
	A	LSW09	1.000		B	LSW18	1.000
六神胶囊	A	LSJN01	0.999	六神胶囊	A	LSJN07	0.998
	A	LSJN02	0.999		A	LSJN08	0.999
	A	LSJN03	1.000		A	LSJN09	0.999
	A	LSJN04	0.999		A	LSJN10	1.000
	A	LSJN05	0.999		A	LSJN11	0.999
	A	LSJN06	0.998		A	LSJN12	1.000

内标液质量浓度/(mg·mL^-1)	对照品质量浓度/(mg·mL^-1)	内标液峰面积	对照品峰面积	校正因子f
0.073 0	0.638 8	35 760.1	387 609.9	10.839 2
0.073 0	0.319 4	33 297.6	164 156.5	4.930 0
0.073 0	0.063 9	30 285.8	23 349.9	0.771 0
0.073 0	0.025 6	31 991.2	7 982.0	0.249 5
0.073 0	0.012 8	33 861.4	6 392.8	0.188 8
0.073 0	0.006 4	24 681.4	1 149.3	0.046 6

剂型	称样量/ g	样品中麝香酮的量/mg	添加麝香酮的量/mg	测出总量/ mg	回收率/ %	平均回收率/%	相对标准偏差/%
六神丸	0.250 0	1.604 6	1.725 9	3.370 7	102.33	102.3	1.0
	0.253 1	1.624 5	1.725 9	3.403 6	103.08
	0.250 9	1.610 4	1.725 9	3.393 4	103.31
	0.251 4	1.613 6	1.725 9	3.394 9	103.21
	0.252 9	1.623 2	1.725 9	3.365 6	100.96
	0.251 6	1.614 9	1.725 9	3.361 3	101.19
六神胶囊	2.006 6	0.488 9	0.517 8	0.992 9	97.33	97.3	1.5
	2.010 6	0.489 9	0.517 8	0.984 5	95.53
	2.035 4	0.496 0	0.517 8	1.008 6	99.02
	2.001 9	0.487 8	0.517 8	1.000 1	98.94
	2.009 8	0.489 7	0.517 8	0.986 1	95.87
	2.010 5	0.489 9	0.517 8	0.992 4	97.04
六神凝胶	7.510 8	0.138 5	0.141 3	0.286 5	104.74	103.1	1.6
	7.500 1	0.138 3	0.141 3	0.285 4	104.11
	7.558 5	0.139 3	0.141 3	0.282 5	101.30
	7.560 5	0.139 4	0.141 3	0.282 6	101.35
	7.483 2	0.137 9	0.141 3	0.286 2	104.90
	7.537 2	0.138 9	0.141 3	0.283 7	102.40

剂型	生产企业	样品编号	麝香酮质量分数/ (mg·g^-1)	剂型	生产企业	样品编号	麝香酮质量分数/ (mg·g^-1)
六神丸	A	LSW01	5.985 5	六神丸	A	LSW10	5.547 5
	A	LSW02	5.857 6		A	LSW11	7.279 5
	A	LSW03	6.046 9		B	LSW12	5.905 3
	A	LSW04	6.277 4		B	LSW13	6.869 6
六神丸	A	LSW05	5.778 4	六神丸	B	LSW14	6.497 4
	A	LSW06	5.694 1		B	LSW15	6.418 4
	A	LSW07	5.963 4		B	LSW16	6.205 7
	A	LSW08	6.702 1		B	LSW17	6.318 2
	A	LSW09	6.557 2		B	LSW18	6.509 3
六神胶囊	A	LSJN01	0.248 6	六神胶囊	A	LSJN07	0.166 2
	A	LSJN02	0.243 7		A	LSJN08	0.233 5
	A	LSJN03	0.112 7		A	LSJN09	0.106 3
	A	LSJN04	0.091 9		A	LSJN10	0.110 2
	A	LSJN05	0.099 7		A	LSJN11	0.092 3
	A	LSJN06	0.161 7		A	LSJN12	0.133 2
六神凝胶	A	LSNJ01	0.020 65	六神凝胶	A	LSNJ06	0.026 05
	A	LSNJ02	0.023 03		A	LSNJ07	0.023 83
	A	LSNJ03	0.021 07		A	LSNJ08	0.018 29
	A	LSNJ04	0.025 52		A	LSNJ09	0.021 72
	A	LSNJ05	0.018 43

[1]	LI Changgeng, LI Junxian, PAN Shaobin, LIU Shuang, KONG Na, DONG Hongjing. The change in volatile compounds of Arecae Semen during stir-frying process based on gas chromatography-ion mobility spectrometry [J]. Shandong Science, 2023, 36(6): 15-21.
[2]	CHEN Xi, GAO Yan, WANG Yanghai, JIA Mingqian, ZHANG Yue, MA Lulan, ZHAO Bonian. Study on the quality standard of vinegar-processed Knoxiae Radix [J]. Shandong Science, 2023, 36(4): 18-28.
[3]	LI Qi-dong,ZHAO Jin,KONG Na,HUANG Lu-yao,PAN Shao-bin. Rapid analysis of the volatile components of Mongolian thyme herb's essential oils using headspace solid-phase microextraction combined with gas chromatography-mass spectrometry [J]. Shandong Science, 2022, 35(1): 1-5.
[4]	XU Yi-zhen. Analysis of volatile oil constitutes of guava leaves by solid phase microextraction [J]. Shandong Science, 2021, 34(6): 15-21.
[5]	LI Li-li, ZHANG Min-min, LI Meng, ZHAO Heng-qiang, GENG Yan-ling. Study of the volatile components in Panax quinquefolius L. with different drying methods [J]. Shandong Science, 2020, 33(3): 62-67.
[6]	SUN Zhi-qiang, WANG Xiao. Quality analysis of Semiaquilegiae Radix of different origins based on haracteristic fingerprint and content determination of two components [J]. Shandong Science, 2020, 33(1): 16-23.
[7]	WANG Xiao, LI Yuan-yuan, SUN Zhi-qiang, WU Ming-ze, GAO Peng, DAI Long. Aesculetin content determination and characteristic HPLC chromatogram of Violae Herba obtained from different habitats [J]. Shandong Science, 2019, 32(4): 24-31.
[8]	LI Yan, CHENG Hong-jie, LI Ke-ming. Content determination of paeoniflorin in Yiganfuzhengqingdu Granules by HPLC [J]. Shandong Science, 2019, 32(2): 22-27.
[9]	SUN Dan-dan, WANG Gang, HE Huan-xiang, GUO Qing-mei. Study on quality of Isatidis Radix in different production areas [J]. SHANDONG SCIENCE, 2018, 31(5): 20-23.
[10]	YAN Hui-jiao, WANG Zhi-wei,LIN Yun-liang, GAO Hong-mei, LI Feng, WANG Xiao, GENG Yan-ling. Quantitative ¹H NMR based content determination of ginsenoside Rd [J]. SHANDONG SCIENCE, 2018, 31(4): 26-30.
[11]	ZHANG Hui，ZHANG Li-mei，LIU Shan-xin，SU Ming，LI Ying，ZHAO Li-jian. Research on determination of ingredients in Dingbai plaster by HPLC [J]. SHANDONG SCIENCE, 2018, 31(3): 19-22.
[12]	YANG Long-fei,DING Xiao-yan,GAO Yan,GUO Jin,SUN Qi-hui,ZHAO Bo-nian. Optimization of water extraction process for Tonglishu Granule by orthogonal experiment [J]. SHANDONG SCIENCE, 2018, 31(1): 23-29.
[13]	LIU Qing, LIU Bo，DING Xiao-yan. Content determination of paeoniflorin in tonic semifluid extract of ten ingredients [J]. SHANDONG SCIENCE, 2017, 30(5): 28-31.
[14]	ZHANG Wei，CAO Jia，WANG Hui，CAO Yun-fei，WANG Wei. Study on in vitro transdermal drug release of Dingjiang Hewei plaster [J]. SHANDONG SCIENCE, 2017, 30(5): 32-36.
[15]	CHI Yu-feng,WANG Xiao-ming,ZHANG Ling,LIN Sha-sha,JIANG Hai-qiang,ZHOU Hong-lei. Simultaneous determination of two alisols in Rhizoma Alismatis by HPLC-MS [J]. SHANDONG SCIENCE, 2017, 30(3): 17-20.

Characteristic chromatograms and content determination of artificial musk in Liushen series preparations based on gas chromatography

RichHTML

PDF (PC)

Like

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 10

References 14

Related Articles 15

Metrics

Comments

Recommended 0