1.广州中医药大学 第五临床医学院,广东 广州 510405
2.广东省中医药工程技术研究院,广东 广州 510095
3.广东省中医药研究开发重点实验室,广东 广州 510095
毕晓黎,博士,主任中药师,研究方向:中药质量评价,E-mail:zyfxyjs@gzucm.edu.cn
收稿:2024-11-22,
修回:2025-01-22,
录用:2025-02-10,
纸质出版:2025-11-15
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贾德政,江洁怡,陈伟韬,张靖年,胥爱丽,谢灿辉,曾志浩,刘焰嫦,肖观林,毕晓黎.煅牡蛎标准汤剂“量-质”传递规律研究[J].分析测试学报,2025,44(11):2265-2276.
JIA De-zheng,JIANG Jie-yi,CHEN Wei-tao,ZHANG Jing-nian,XU Ai-li,XIE Can-hui,ZENG Zhi-hao,LIU Yan-chang,XIAO Guan-lin,BI Xiao-li.Research on the Law of“Quantity-Quality”Transfer of the Standard Decoction of Calcined Ostreae Concha[J].Journal of Instrumental Analysis,2025,44(11):2265-2276.
贾德政,江洁怡,陈伟韬,张靖年,胥爱丽,谢灿辉,曾志浩,刘焰嫦,肖观林,毕晓黎.煅牡蛎标准汤剂“量-质”传递规律研究[J].分析测试学报,2025,44(11):2265-2276. DOI: 10.12452/j.fxcsxb.241122552.
JIA De-zheng,JIANG Jie-yi,CHEN Wei-tao,ZHANG Jing-nian,XU Ai-li,XIE Can-hui,ZENG Zhi-hao,LIU Yan-chang,XIAO Guan-lin,BI Xiao-li.Research on the Law of“Quantity-Quality”Transfer of the Standard Decoction of Calcined Ostreae Concha[J].Journal of Instrumental Analysis,2025,44(11):2265-2276. DOI: 10.12452/j.fxcsxb.241122552.
综合运用现代分析方法,以出膏率、CaCO
3
含量、CaCO
3
转移率,以及同步热分析(TG-DSC)、傅里叶变换红外光谱(FTIR)、高效液相色谱(HPLC)指纹图谱为关键质量属性,揭示牡蛎药材-煅牡蛎饮片-煅牡蛎标准汤剂的“量-质”传递规律,为其质量控制提供参考。选取15批牡蛎药材为原料,制备煅牡蛎饮片及煅牡蛎标准汤剂,计算煅牡蛎标准汤剂出膏率,采用络合滴定法测定三者CaCO
3
含量,计算煅牡蛎饮片-标准汤剂CaCO
3
转移率;采用TG-DSC研究三者的热分解特性及热效应特征,构建TG-DSC指纹图谱;采用FTIR建立FTIR指纹图谱,剖析三者化学基团的动态变化情况;采用HPLC测定三者的氨基酸成分,构建HPLC指纹图谱,并进行相似度评价。同时结合主成分分析(PCA)、偏最小二乘法-判别分析(PLS-DA)探寻三者在FTIR特征以及氨基酸成分方面的异同。结果显示,15批牡蛎药材、煅牡蛎饮片及煅牡蛎标准汤剂CaCO
3
含量分别为94.68%~97.79%、96.53%~98.41%、81.86%~90.21%,煅牡蛎标准汤剂出膏率为2.78%~4.94%,煅牡蛎饮片-标准汤剂的CaCO
3
转移率为2.54%~4.42%;TG-DSC结果表明,三者有机质及CaCO
3
分别在30~580 ℃、580~800 ℃范围内分解,且与药材、饮片相比,煅牡蛎标准汤剂中CaCO
3
吸热峰提前,热稳定性显著降低;FTIR结果表明,三者主要成分均为方解石型CaCO
3
,牡蛎药材中主要存在O—H、C=O及CO
3
2-
基团,煅制后未见C=O基团;HPLC结果表明,所建立的指纹图谱平均相似度均在0.9以上,14种氨基酸成分可有效传递。此外,多元统计分析方法可有效将三者区分,筛选出7个FTIR差异波段、3种氨基酸差异成分。所建立的方法可用于煅牡蛎标准汤剂全过程的质
量控制。
By comprehensively applying modern analytical methods,taking the extract yield,the content of CaCO
3
,the transfer rate of CaCO
3
,as well as simultaneous thermal analysis(TG-DSC),Fourier transform infrared spectroscopy(FTIR),and high performance liquid chromatography(HPLC) fingerprints as key quality attributes,this study reveals the“quantity-quality”transfer rules of
Ostreae concha
,calcined slices of
Ostreae concha
,and the standard decoction of calcined
Ostreae concha
,providing a reference for their quality control. Fifteen batches of
Ostreae concha
medicinal materials were selected as raw materials to prepare the calcined slices of
Ostreae concha
and the standard decoction of calcined
Ostreae concha
. The extract yield of the standard decoction of calcined
Ostreae concha
was calculated. The complexometric titration method was used to determine the CaCO
3
content of the three,and the transfer rate of CaCO₃ from the calcined slices of
Ostreae concha
to the standard decoction was calculated. TG-DSC was used to study the thermal decomposition characteristics and thermal effect characteristics of the three,and TG-DSC fingerprints were constructed. FTIR was used to establish FTIR fingerprints to analyze the dynamic changes of chemical groups in the three. HPLC was used to determine the amino acid components of the three,and HPLC fingerprints were constructed,and similarity evaluation was carried out. At the same time,combined with principal component analysis(PCA) and partial least squares-discriminant analysis(PLS-DA),the similarities and differences among the three in terms of FTIR characteristics and amino acid components were explored. The results showed that the CaCO
3
contents of 15 batches of
Ostreae concha
,calcined slices of
Ostreae concha
,and the standard decoction of calcined
Ostreae concha
were 94.68%-97.79%,96.53%-98.41%,and 81.86%-90.21%,respectively. The extract yield of the standard decoction of calcined
Ostreae concha
was 2.78%-4.94%,and the transfer rate of CaCO
3
from the calcined slices of
Ostreae concha
to the standard decoction was 2.54%-4.42%. The results of TG-DSC showed that the organic components and CaCO
3
in
Ostreae concha
,the calcined slices of
Ostreae concha
and the standard decoction of calcined
Ostreae concha
decomposed within the temperature ranges of 30-580 ℃ and 580-800 ℃ respectively. Compared with
Ostreae concha
and the calcined slices of
Ostreae concha
,the endothermic peak of CaCO
3
in the standard decoction of calcined
Ostreae concha
appeared earlier,and its thermal stability decreased significantly. The FTIR results showed that the main component of the three was calcite-type CaCO
3
. The main groups in
Ostreae concha
were O—H,C=O,and CO
3
2-
groups,and the C=O group was not observed after calcination. The HPLC results showed that the average similarity of the established fingerprints was all above 0.9,and 14 amino acid components could be effectively transferred. In addition,the multivariate statistical analysis method could effectively distinguish the three,and 7 FTIR differential bands and 3 amino acid differential components were screened out. The method established in this study can be used for the quality control of the whole process of the standard decoction of calcined
Ostreae concha
.
Chen S L , Liu A , Li Q , Shan T X , Zhu G W , Sun Y , Dai Y T , Zhang J , Zhang T J , You T J J , Liu C X . China J. Chin. Mater. Med. (陈士林,刘安,李琦,杉田享,朱广伟,孙奕,代云桃,章军,张铁军,友田健久,刘昌孝. 中国中药杂志), 2016 , 41 ( 8 ): 1367 - 1375 .
Du J C , Pu X L , Fan K L , Zhai Y J , Zhang Y J , Wang X H , Chen S J , Li S , Zhang Y T , Chen K J , Peng J , Xu Y M . China J. Chin. Mater. Med. (杜俊潮,浦香兰,范恺磊,翟燕娟,张宇静,王协和,陈盛君,李松,张云天,陈可冀,彭军,许运明. 中国中药杂志), 2020 , 45 ( 20 ): 4909 - 4917 .
Geng S L , Zhou Q , Sun S G , Li M , Zhao L J , Zhang J Q , Feng Y . Chin. Tradit. Pat. Med. (耿赛龙,周琴,孙水根,李曼,赵立杰,张继全,冯怡. 中成药), 2024 , 46 ( 2 ): 370 - 378 .
Jiang X Y , Liu X M , Wang X , Ma J M , Tian W , Niu L Y . Hebei J. Ind. Sci. Technol. (姜晓娅,刘晓明,王相,麻景梅,田伟,牛丽颖. 河北工业科技), 2024 , 41 ( 5 ): 367 - 375 .
Yu X H , Cao S , Xin L , Ji Q , He Y J , Ma Y M , Zhu S , Xu L . Jiangxi Chem. Ind. (于现花,曹帅,信龄,季前,贺宇洁,马翊铭,朱帅,徐蕾. 江西化工), 2024 , 40 ( 5 ): 8 - 13,17 .
Zhu H J , Lu Z M , Lin H T . China ’ s Naturopathy (祝恒健,卢转明,林惠婷 . 中国民间疗法) , 2024 , 32 ( 9 ): 28 - 30 .
Zhong Y R , Zhu H C , He M Y , Wen S Q , Chen J , Zhong S . Chin. J. Clin. Ration. Drug Use (钟宇汝,朱虹春,和明扬,文思棋,陈婧,钟森. 临床合理用药), 2024 , 17 ( 5 ): 31 - 36,47 .
Zhuang Y X , Lu Y N , Hu J W , Zhang Y Q , Meng J , Zhan Z L , Yang C Z . Chin. J. Exp. Tradit. Med. Formulae (庄怡雪,陆一南,胡静雯,张艺勤,孟静,詹志来,杨成梓. 中国实验方剂学杂志), 2023 , 29 ( 6 ): 25 - 33 .
Liu S J , Wu S C , Ma Y L , Zhao Q , Ao W L J , Wang X X , Duan J A . Chin. Tradit. Herb. Drugs(刘圣金 , 吴思澄 , 马瑜璐 , 赵倩 , 奥·乌力吉 , 王秀秀 , 段金廒 . 中草药) , 2023 , 54 ( 19 ): 6555 - 6568 .
Chinese Pharmacopoeia Commission . Pharmacopoeia of the People ’ s Republic of China . Part Ⅰ. 2020 ed. Beijing : China Medical Science Press(国家药典委员会. 中华人民共和国药典. 一部. 2020版. 北京:中国医药科技出版社) , 2020 : 180 - 181 .
Wu L Z , Guo R , Zhu Y Y , Liu X , Li W D , Cai B C , Qin K M . J. Chin. Med. Mater. (吴丽竹,郭溶,祝溢阳,刘晓,李伟东,蔡宝昌,秦昆明. 中药材), 2024 , 47 ( 3 ): 774 - 778 .
Zhao S Y , Wu N , Sun J M , Zhang H . Jilin J . Chin. Med. (赵思远,吴楠,孙佳明,张辉. 吉林中医药), 2014 , 34 ( 8 ): 821 - 824 .
Zhao Y Y , Wei F H , Wang Y L . Chin . J. Exp. Tradit. Med. Formulae (赵玉英,魏凤华,王颖莉. 中国实验方剂学杂志), 2014 , 20 ( 12 ): 110 - 114 .
Cao S W , Xiang S J , Wu W F , Ruan S F , Wang Z X , Liu L , Shen Q , Chen H J , Weng L D , Zhu H X , An B C , Liu Q . Chin. J. Exp. Tradit. Med. Formulae (曹思玮,乡世健,吴文锋,阮世发,王著显,刘莉,沈群,陈活记,翁立冬,朱红霞,安佰超,刘强. 中国实验方剂学杂志), 2018 , 24 ( 16 ): 7 - 11 .
Chinese Pharmacopoeia Commission . Pharmacopoeia of the People ’ s Republic of China . Part Ⅳ. 2020 ed. Beijing : China Medical Science Press(国家药典委员会. 中华人民共和国药典. 四部. 2020版. 北京:中国医药科技出版社) , 2020 : 29 - 34 .
National Administration of Traditional Chinese Medicine . Announcement No . 3 [2009] of Management Specifications for Traditional Chinese Medicine Decoction Rooms in Medical Institutions(国家中医药管理局. 《医疗机构中药煎药室管理规范》2009 年第 3 号公告) . [ 2009-03-16 ]. http://www.natcm.gov.cn/yizhengsi/gongzuodongtai/2018-03-25/6577.html http://www.natcm.gov.cn/yizhengsi/gongzuodongtai/2018-03-25/6577.html .
National Medical Products Administration . Announcement No . 16 [2021]of Technical Requirements for Quality Control and Standard Establishment of Traditional Chinese Medicine Formula Granules(国家药品监督管理局. 《中药配方颗粒质量控制与标准制定技术要求》2021年第16号通告) . [ 2021-01-26 ]. https://www.gov.cn/zhengce/zhengceku/2021-02/11/content_5586817.htm https://www.gov.cn/zhengce/zhengceku/2021-02/11/content_5586817.htm .
Shi Z J , Chen L M , Jiang T , Weng Y P , Xu P S , Chen J C . Strait Pharm. J. (施枝江,陈林明,姜涛,翁玉萍, 许沛森,陈锦淳. 海峡药学), 2020 , 32 ( 9 ): 69 - 71 .
Yang G C , Yang Y F , Xu S E , Ke J , Chen L Y , Hou A G , Jin W B . Chin. Tradit. Pat. Med. (杨国春,杨亚芳,徐素娥,柯瑾,陈凌云,侯安国,金文彬. 中成药), 2024 , 46 ( 6 ): 1773 - 1781 .
Hao L P , Yu L H , Gao W Y , Yan S , Liu G S , Hao H S . J. Dalian Polytech. Univ. (郝丽萍,俞莉红,高文元,闫爽,刘贵山,郝洪顺. 大连工业大学学报), 2020 , 39 ( 3 ): 220 - 224 .
Lin L J . Guangzhou Chem. Ind. (林丽君. 广州化工), 2020 , 48 ( 6 ): 101 - 103 .
Yue G Y , Sun Z Q , Wang B L , Zhou F Q , Guo Q M , Sun Z Y . Chin. J. Mar. Drugs (岳改月,孙昭倩,王百龙,周凤琴,郭庆梅,孙稚颖. 中国海洋药物), 2021 , 40 ( 1 ): 37 - 40 .
Yang L , Li X L , Zhao Z C , Chen L , Li M , Zhang X M , Liu Y P , Chen H P . Lishizhen Med. Mater. Med. Res . (杨丽,李雪莲,赵梓辰,陈林,李旻,张小梅, 刘友平,陈鸿平. 时珍国医国药), 2014 , 25 ( 10 ): 2412 - 2414 .
Wu R , Liu Z X , Huang H W , Yan J , Liu Y . Chin. J. Pharm. Anal. (吴锐,刘朝霞,黄海伟,严菁,刘毅. 药物分析杂志), 2020 , 40 ( 8 ): 1494 - 1502 .
Zeng X P , Wu B , Jiang S , Deng X R . Guangdong Chem. Ind. (曾小平,吴冰,江山,邓雪蓉. 广东化工), 2010 , 37 ( 5 ): 70 - 72 .
Weng S F . Fourier Transform Infrared Spectroscopy . 2nd ed . Beijing : Chemical Industry Press (翁诗甫. 傅里叶变换红外光谱分析. 2版. 北京:化学工业出版社) , 2012 : 304 .
Fan L W , Yang M X . J . Mineral. Petrol. (范陆薇,杨明星. 矿物岩石), 2010 , 30 ( 2 ): 21 - 24 .
Zhang B , Xiao X , Han Y J , Zhang Y Y , Yu H W . Inorg. Chem. Ind. (张彬,肖霄,韩芸娇,张媛媛,于宏伟. 无机盐工业), 2021 , 53 ( 1 ): 97 - 101 .
Yang N , Kuang S Y , Yue Y H . J . Mineral. Petrol. (杨念,况守英,岳蕴辉. 矿物岩石), 2015 , 35 ( 4 ): 37 - 42 .
Guo Y F , Cao Q , Ye L L , Zhang C Y , Kou R B , Wang J M , Guo M . Spectrosc. Spectral Anal. (郭亚菲,曹强,叶蕾蕾,张成园,寇仁博,王君梅,郭玫. 光谱学与光谱分析), 2024 , 44 ( 1 ): 188 - 196 .
Liu Y , Chen W F , Wang J R , Liu H M , Fang C X , Guo L . J. Chin. Med. Mater. (刘宇,陈文仿,王江瑞,刘红梅,方成鑫,郭力. 中药材), 2016 , 39 ( 12 ): 2733 - 2737 .
Liu Z J , Bi F J , Lin T . J. Instrum. Anal. (刘主洁,毕福钧,林彤. 分析测试学报), 2024 , 43 ( 11 ): 1835 - 1842 .
Jin Q , Sun X F , Tang W , Hu Y X , Luo L , Lu F , Liao H Y . J. Instrum. Anal. (金强,孙学锋,唐伟,胡玉轩,罗亮,陆飞,廖惠云. 分析测试学报), 2024 , 43 ( 4 ): 574 - 581 .
Qin L Y , Liang L J , Hu Y , Gan L F , Huang S , Xu J , Zhang Z P . Chin. Tradit. Herb. Drugs (覃柳莹,梁丽金,胡懿,甘力帆,黄森,徐杰,张志鹏. 中草药), 2023 , 54 ( 18 ): 5892 - 5903 .
Jia M T , Li C Y , Qiang Z Z , Feng H M , Li Y , Luo X D , Liang T T . Chin. J. Tradit. Chin. Med. Pharm. (贾妙婷,李成义,强正泽,冯慧敏,李玥,罗旭东,梁婷婷. 中华中医药杂志), 2023 , 38 ( 7 ): 3054 - 3059 .
Yu X T , Cao Q , Zhang L L , Wang K D , Chen Z S , Pan L , Zhang Z . Chin. Pharm. J. (余欣彤,曹嵌,张兰兰,汪凯东,陈灶树,潘玲,张正. 中国药学杂志), 2024 , 59 ( 22 ): 2132 - 2139 .
Liao N X , Shi D Z , Xiao L L , Liu H L , Xie Y X , Yang Z Q , Zhao M , Zheng C , Zhu Y B , Hu Y , Cheng J M . Chin. Tradit. Herb. Drugs (廖楠汐,石德志,肖莲莲,刘华兰,解雨欣,杨正清,赵勉,郑超,朱喻波,胡杨,程建明. 中草药), 2024 , 55 ( 18 ): 6355 - 6362 .
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