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Article(id=1256183373366739849, tenantId=1146029695717560320, journalId=1255847919539208197, issueId=1256183358493679805, articleNumber=null, orderNo=null, doi=10.13193/j.issn.1673-7717.2025.12.029, 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=null, acceptedDateStr=null, onlineDate=1777427054968, onlineDateStr=2026-04-29, pubDate=1765296000000, pubDateStr=2025-12-10, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1777427054968, onlineIssueDateStr=2026-04-29, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1777427054968, creator=13701087609, updateTime=1777427054968, updator=13701087609, issue=Issue{id=1256183358493679805, tenantId=1146029695717560320, journalId=1255847919539208197, year='2025', volume='43', issue='12', pageStart='1', pageEnd='258', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1777427051344, creator=13701087609, updateTime=1777427760067, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1256186331126969089, tenantId=1146029695717560320, journalId=1255847919539208197, issueId=1256183358493679805, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1256186331126969090, tenantId=1146029695717560320, journalId=1255847919539208197, issueId=1256183358493679805, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=162, endPage=167, ext={EN=ArticleExt(id=1256183378504762296, articleId=1256183373366739849, tenantId=1146029695717560320, journalId=1255847919539208197, language=EN, title=Research on Identification Method of Shicangpu（Acori Tatarinowii Rhizoma）and Common Counterfeits Based on Ultra-High Performance Liquid Chromatography, columnId=1256183361521967297, journalTitle=Chinese Archives of Traditional Chinese Medicine, columnName=Target on National Project, runingTitle=null, highlight=null, articleAbstract=
Objective

To establish amethod for identifying Shicangpu（Acori Tatarinowii Rhizoma）（ATR）from common counterfeits by ultra performance liquid chromatography（UPLC）technology，and to provide reference for quality evaluation and control of ATR.

Methods

Waters CORTECST3 column（2.1 mm×150 mm，1.6μm）was used.Methanol：acetonitrile 1：1（A）-water（B）solution was used as mobile phase and gradientelution was performed.The flow ratewas0.2mL/min.The column temperature was40℃.The detection wavelength was275 nm and the sample volume was3μL.The UPLC characteristic map was established to identify ATR from common counterfeits.

Results

The UPLC characteristic map identified 4 common peaks of ATR and identified 1 of them.The similarity among samples was 0.892～0.996.

Conclusion

The established method of characteristic map is simple，reliable，accurate and repeatable，which can identify the authenticity of ATR directly，provide a specific method for the quality control and authenticity identification of ATR，and effectively improve the drug safety of related products.

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目的

采用超高效液相色谱（UPLC）技术建立石菖蒲与常见伪品的鉴别方法，为石菖蒲药材的质量评价和控制提供参考。

方法

采用Waters CORTECST3（2.1 mm×150 mm，1.6μm）色谱柱；将甲醇∶乙腈＝1∶1（A）-水（B）溶液作为流动相，梯度洗脱；流速为0.2 mL/min；柱温设置在40℃；在275 nm波长处检测，进样体积3μL，建立UPLC特征图谱，对石菖蒲药材与常见伪品进行鉴别。

结果

实验建立的UPLC特征图谱确定了石菖蒲4个共有峰并指认其中1个峰，石菖蒲样品间相似度在0.892～0.996。

结论

建立的特征图谱方法简便可靠，精密度、重复性良好，可以直观地判断石菖蒲药材的真伪，为石菖蒲药材质量控制、真伪鉴别提供具有专属性的方法，有效提高石菖蒲相关产品用药安全。

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谭晓梅（1963-），女，湖南澧县人，研究员，博士研究生导师，博士，研究方向：中药新制剂及中药复方配伍规律。Email：。
陈向东（1975-），男，广东梅州人，教授，硕士研究生导师，硕士，研究方向：中药饮片及中药配方颗粒。E-mail：。
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邓香华（1997-），女，广东茂名人，硕士，研究方向：中药饮片及中药配方颗粒。

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邓香华（1997-），女，广东茂名人，硕士，研究方向：中药饮片及中药配方颗粒。

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样品名称批号产地样品名称批号产地
石菖蒲ATR-1江西省石菖蒲ATR-18江西省
ATR-2湖北省ATR-19江西省
ATR-3安徽省ATR-20安徽省
ATR-4安徽省茴香菖蒲AGR-1贵州省
ATR-5安徽省AGR-2贵州省
ATR-6安徽省AGR-3贵州省
ATR-7安徽省AGR-4贵州省
ATR-8安徽省水菖蒲ACR-1山东省
ATR-9安徽省ACR-2湖南省
ATR-10安徽省ACR-3湖北省
ATR-11安徽省九节菖蒲AAR-1广西
ATR-12四川省AAR-2甘肃省
ATR-13四川省AAR-3陕西省
ATR-14四川省AAR-4甘肃省
ATR-15江西省岩白菜BPR-1云南省
ATR-16江西省BPR-2安徽省
ATR-17江西省BPR-3云南省
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样品来源信息

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样品名称批号产地样品名称批号产地
石菖蒲ATR-1江西省石菖蒲ATR-18江西省
ATR-2湖北省ATR-19江西省
ATR-3安徽省ATR-20安徽省
ATR-4安徽省茴香菖蒲AGR-1贵州省
ATR-5安徽省AGR-2贵州省
ATR-6安徽省AGR-3贵州省
ATR-7安徽省AGR-4贵州省
ATR-8安徽省水菖蒲ACR-1山东省
ATR-9安徽省ACR-2湖南省
ATR-10安徽省ACR-3湖北省
ATR-11安徽省九节菖蒲AAR-1广西
ATR-12四川省AAR-2甘肃省
ATR-13四川省AAR-3陕西省
ATR-14四川省AAR-4甘肃省
ATR-15江西省岩白菜BPR-1云南省
ATR-16江西省BPR-2安徽省
ATR-17江西省BPR-3云南省
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序号名称保留时间（min）/面积/
（mAU·min）		分离度理论塔板数
1峰110.812668 634-119 905
2峰215.767312 52030.13492 115
3峰3（β-细辛醚）20.5914 523 49429.466437 796
4峰420.9212 089 1992.779512 415
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专属性结果

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序号名称保留时间（min）/面积/
（mAU·min）		分离度理论塔板数
1峰110.812668 634-119 905
2峰215.767312 52030.13492 115
3峰3（β-细辛醚）20.5914 523 49429.466437 796
4峰420.9212 089 1992.779512 415
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石菖蒲样品峰1峰2峰3（β-细辛醚）峰4
ATR-10.0840.0151.0000.038
ATR-20.1130.0191.0000.044
ATR-30.0700.0551.0000.257
ATR-40.2320.4051.0000.595
ATR-50.0670.0271.0000.214
ATR-60.0800.0161.0000.055
ATR-70.0390.0111.0000.119
ATR-80.1660.0201.0000.024
ATR-90.0930.0101.0000.080
ATR-100.1530.0221.0000.048
ATR-110.0460.0601.0000.270
ATR-120.0980.1701.0000.284
ATR-130.1960.1651.0000.342
ATR-140.2740.0481.0000.052
ATR-150.3800.0561.0000.033
ATR-160.5970.0901.0000.027
ATR-170.2120.0371.0000.049
ATR-180.1510.0741.0000.460
ATR-190.2580.0631.0000.040
ATR-200.3360.1031.0000.104
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石菖蒲药材特征图谱共有峰相对峰面积

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石菖蒲样品峰1峰2峰3（β-细辛醚）峰4
ATR-10.0840.0151.0000.038
ATR-20.1130.0191.0000.044
ATR-30.0700.0551.0000.257
ATR-40.2320.4051.0000.595
ATR-50.0670.0271.0000.214
ATR-60.0800.0161.0000.055
ATR-70.0390.0111.0000.119
ATR-80.1660.0201.0000.024
ATR-90.0930.0101.0000.080
ATR-100.1530.0221.0000.048
ATR-110.0460.0601.0000.270
ATR-120.0980.1701.0000.284
ATR-130.1960.1651.0000.342
ATR-140.2740.0481.0000.052
ATR-150.3800.0561.0000.033
ATR-160.5970.0901.0000.027
ATR-170.2120.0371.0000.049
ATR-180.1510.0741.0000.460
ATR-190.2580.0631.0000.040
ATR-200.3360.1031.0000.104
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茴香菖蒲样品峰1峰5峰6峰2峰3（β-细辛醚）峰4
AGR-10.2311.1450.3230.2391.0000.012
AGR-20.1100.3570.0620.1091.0000.023
AGR-30.1310.5490.1570.1161.0000.018
AGR-40.1460.4380.0740.1371.0000.034
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茴香菖蒲药材特征图谱共有峰相对峰面积

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茴香菖蒲样品峰1峰5峰6峰2峰3（β-细辛醚）峰4
AGR-10.2311.1450.3230.2391.0000.012
AGR-20.1100.3570.0620.1091.0000.023
AGR-30.1310.5490.1570.1161.0000.018
AGR-40.1460.4380.0740.1371.0000.034
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水菖蒲峰1峰2峰7峰8峰3（β-细辛醚）峰4
ACR-10.1860.0380.0440.0451.0000.076
ACR-20.1220.0140.0220.0271.0000.075
ACR-30.2770.0470.0520.0431.0000.112
), ArticleFig(id=1256183489880309953, tenantId=1146029695717560320, journalId=1255847919539208197, articleId=1256183373366739849, language=CN, label=表5, caption=

水菖蒲药材特征图谱共有峰相对峰面积

, figureFileSmall=null, figureFileBig=null, tableContent=
水菖蒲峰1峰2峰7峰8峰3（β-细辛醚）峰4
ACR-10.1860.0380.0440.0451.0000.076
ACR-20.1220.0140.0220.0271.0000.075
ACR-30.2770.0470.0520.0431.0000.112
), ArticleFig(id=1256183490719170760, tenantId=1146029695717560320, journalId=1255847919539208197, articleId=1256183373366739849, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称峰9-峰面积样品名称峰9-峰面积
AAR-113 925BPR-126 844
AAR-230 789BPR-239 824
AAR-321 690BPR-321 899
AAR-423 730--
), ArticleFig(id=1256183491402842320, tenantId=1146029695717560320, journalId=1255847919539208197, articleId=1256183373366739849, language=CN, label=表6, caption=

九节菖蒲与岩白菜药材特征图谱共有峰峰面积

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称峰9-峰面积样品名称峰9-峰面积
AAR-113 925BPR-126 844
AAR-230 789BPR-239 824
AAR-321 690BPR-321 899
AAR-423 730--
), ArticleFig(id=1256183492027793622, tenantId=1146029695717560320, journalId=1255847919539208197, articleId=1256183373366739849, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称相似度样品名称相似度
ATR-10.985ATR-180.986
ATR-20.994ATR-190.991
ATR-30.965ATR-200.978
ATR-40.909AGR-10.938
ATR-50.991AGR-20.986
ATR-60.995AGR-31.000
ATR-70.993AGR-40.995
ATR-80.963ACR-10.994
ATR-90.996ACR-21.000
ATR-100.978ACR-30.999
ATR-110.892AAR-11.000
ATR-120.992AAR-21.000
ATR-130.986AAR-31.000
ATR-140.993AAR-41.000
ATR-150.990BPR-11.000
ATR-160.994BPR-21.000
ATR-170.996BPR-31.000
), ArticleFig(id=1256183492459806940, tenantId=1146029695717560320, journalId=1255847919539208197, articleId=1256183373366739849, language=CN, label=表7, caption=

石菖蒲、茴香菖蒲、水菖蒲、九节菖蒲、岩白菜药材特征图谱相似度评价结果

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样品名称相似度样品名称相似度
ATR-10.985ATR-180.986
ATR-20.994ATR-190.991
ATR-30.965ATR-200.978
ATR-40.909AGR-10.938
ATR-50.991AGR-20.986
ATR-60.995AGR-31.000
ATR-70.993AGR-40.995
ATR-80.963ACR-10.994
ATR-90.996ACR-21.000
ATR-100.978ACR-30.999
ATR-110.892AAR-11.000
ATR-120.992AAR-21.000
ATR-130.986AAR-31.000
ATR-140.993AAR-41.000
ATR-150.990BPR-11.000
ATR-160.994BPR-21.000
ATR-170.996BPR-31.000
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样品名称峰面积/（mAU·min）总峰面积/（mAU·min）称样量/（g）总峰面积/称样量峰3面积百分比/（%）
峰1峰2峰3（S）峰4
加水10 mL155 31399 578799 779332 0421 386 7121.01101 371 62457.67
加水20 mL407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
加水30 mL502 863417 3107 118 3163 082 07311 120 5621.001 311 106 12464.01
煎煮15 min348 721303 6942 690 435917 5254 260 3751.015 64 194 93463.15
煎煮30 min389 289318 6164 793 5342 194 8077 696 2461.015 87 576 53762.28
煎煮60 min407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
煎煮90 min339 344279 2122 578 0201 047 3994 243 9751.013 54 187 44460.75
萃取2次337 657299 7104 505 0402 149 5487 291 9551.008 77 229 06261.78
萃取3次407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
萃取4次237 191182 0282 899 8871 394 8194 713 9251.009 54 669 56461.52
萃取体积10 mL338 155293 9903 779 8641 707 4786 119 4871.016 56 020 15461.77
萃取体积20 mL407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
萃取体积30 mL409 986285 0832 631 4251 091 7984 418 2921.009 94 374 98059.56
0%甲醇复溶529 531209 1022 710 6681 214 1654 663 4661.001 04 658 80758.13
30%甲醇复溶518 431142 4554 687 7242 020 1807 368 7901.000 97 362 16463.62
50%甲醇复溶714 081256 6624 469 5731 717 5617 157 8771.004 47 126 52062.44
70%甲醇复溶407 698321 8094 355 7192 000 0987 085 3241.009 47 019 34261.48
100%甲醇复溶792 577287 7905 978 3912 586 6619 645 4191.006 39 585 03361.98
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样品制备条件考察结果

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称峰面积/（mAU·min）总峰面积/（mAU·min）称样量/（g）总峰面积/称样量峰3面积百分比/（%）
峰1峰2峰3（S）峰4
加水10 mL155 31399 578799 779332 0421 386 7121.01101 371 62457.67
加水20 mL407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
加水30 mL502 863417 3107 118 3163 082 07311 120 5621.001 311 106 12464.01
煎煮15 min348 721303 6942 690 435917 5254 260 3751.015 64 194 93463.15
煎煮30 min389 289318 6164 793 5342 194 8077 696 2461.015 87 576 53762.28
煎煮60 min407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
煎煮90 min339 344279 2122 578 0201 047 3994 243 9751.013 54 187 44460.75
萃取2次337 657299 7104 505 0402 149 5487 291 9551.008 77 229 06261.78
萃取3次407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
萃取4次237 191182 0282 899 8871 394 8194 713 9251.009 54 669 56461.52
萃取体积10 mL338 155293 9903 779 8641 707 4786 119 4871.016 56 020 15461.77
萃取体积20 mL407 802319 8694 357 2191 999 0897 083 9791.009 47 018 01061.51
萃取体积30 mL409 986285 0832 631 4251 091 7984 418 2921.009 94 374 98059.56
0%甲醇复溶529 531209 1022 710 6681 214 1654 663 4661.001 04 658 80758.13
30%甲醇复溶518 431142 4554 687 7242 020 1807 368 7901.000 97 362 16463.62
50%甲醇复溶714 081256 6624 469 5731 717 5617 157 8771.004 47 126 52062.44
70%甲醇复溶407 698321 8094 355 7192 000 0987 085 3241.009 47 019 34261.48
100%甲醇复溶792 577287 7905 978 3912 586 6619 645 4191.006 39 585 03361.98
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基于超高效液相色谱技术的石菖蒲与常见伪品鉴别方法研究
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邓香华 1, 2 , 孙冬梅 2 , 谭晓梅 1 , 贾小舟 2 , 罗穆祥 1, 2 , 夏天睿 2 , 李国卫 2 , 陈向东 2
中华中医药学刊 | 国家项目点击 2025,43(12): 162-167
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中华中医药学刊 | 国家项目点击 2025, 43(12): 162-167
基于超高效液相色谱技术的石菖蒲与常见伪品鉴别方法研究
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邓香华1, 2, 孙冬梅2, 谭晓梅1 , 贾小舟2, 罗穆祥1, 2, 夏天睿2, 李国卫2, 陈向东2
作者信息
  • 1.南方医科大学中医药学院，广东省中药制剂重点实验室，广东 广州 510515
  • 2.广东一方制药有限公司，广东省中药配方颗粒企业重点实验室，广东 佛山 528244

    • 邓香华（1997-），女，广东茂名人，硕士，研究方向：中药饮片及中药配方颗粒。

通讯作者:

谭晓梅（1963-），女，湖南澧县人，研究员，博士研究生导师，博士，研究方向：中药新制剂及中药复方配伍规律。Email：。
陈向东（1975-），男，广东梅州人，教授，硕士研究生导师，硕士，研究方向：中药饮片及中药配方颗粒。E-mail：。
Research on Identification Method of Shicangpu（Acori Tatarinowii Rhizoma）and Common Counterfeits Based on Ultra-High Performance Liquid Chromatography
Xianghua DENG1, 2, Dongmei SUN2, Xiaomei TAN1 , Xiaozhou JIA2, Muxiang LUO1, 2, Tianrui XIA2, Guowei LI2, Xiangdong CHEN2
Affiliations
  • 1.College of Traditional Chinese Medicine，Southern Medical University/Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Preparations，Guangzhou 510515，Guangdong，China
  • 2.Guangdong Yifang Pharmaceutical Co.，Ltd/Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Formula，Foshan 528244，Guangdong，China
出版时间: 2025-12-10 doi: 10.13193/j.issn.1673-7717.2025.12.029
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摘要
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目的

采用超高效液相色谱（UPLC）技术建立石菖蒲与常见伪品的鉴别方法，为石菖蒲药材的质量评价和控制提供参考。

方法

采用Waters CORTECST3（2.1 mm×150 mm，1.6μm）色谱柱；将甲醇∶乙腈＝1∶1（A）-水（B）溶液作为流动相，梯度洗脱；流速为0.2 mL/min；柱温设置在40℃；在275 nm波长处检测，进样体积3μL，建立UPLC特征图谱，对石菖蒲药材与常见伪品进行鉴别。

结果

实验建立的UPLC特征图谱确定了石菖蒲4个共有峰并指认其中1个峰，石菖蒲样品间相似度在0.892～0.996。

结论

建立的特征图谱方法简便可靠，精密度、重复性良好，可以直观地判断石菖蒲药材的真伪，为石菖蒲药材质量控制、真伪鉴别提供具有专属性的方法，有效提高石菖蒲相关产品用药安全。

石菖蒲  /  水（藏）菖蒲  /  茴香（金钱）菖蒲  /  九节菖蒲  /  岩白菜  /  UPLC  /  鉴别
Objective

To establish amethod for identifying Shicangpu（Acori Tatarinowii Rhizoma）（ATR）from common counterfeits by ultra performance liquid chromatography（UPLC）technology，and to provide reference for quality evaluation and control of ATR.

Methods

Waters CORTECST3 column（2.1 mm×150 mm，1.6μm）was used.Methanol：acetonitrile 1：1（A）-water（B）solution was used as mobile phase and gradientelution was performed.The flow ratewas0.2mL/min.The column temperature was40℃.The detection wavelength was275 nm and the sample volume was3μL.The UPLC characteristic map was established to identify ATR from common counterfeits.

Results

The UPLC characteristic map identified 4 common peaks of ATR and identified 1 of them.The similarity among samples was 0.892～0.996.

Conclusion

The established method of characteristic map is simple，reliable，accurate and repeatable，which can identify the authenticity of ATR directly，provide a specific method for the quality control and authenticity identification of ATR，and effectively improve the drug safety of related products.

Shichangpu（Acori Tatarinowii Schott）  /  Shuicangpu（Acorus calamus L.）  /  Huixiang Changpu（Acorus gramineus Soland）  /  Jiujie Changpu（Anemone altaica Fisch）  /  Yanbaicai［Bergenia purpurascens（Hook.f.et Thoms.）Engl.］  /  UPLC  /  identification
邓香华, 孙冬梅, 谭晓梅, 贾小舟, 罗穆祥, 夏天睿, 李国卫, 陈向东. 基于超高效液相色谱技术的石菖蒲与常见伪品鉴别方法研究. 中华中医药学刊, 2025 , 43 (12) : 162 -167 . DOI: 10.13193/j.issn.1673-7717.2025.12.029
Xianghua DENG, Dongmei SUN, Xiaomei TAN, Xiaozhou JIA, Muxiang LUO, Tianrui XIA, Guowei LI, Xiangdong CHEN. Research on Identification Method of Shicangpu（Acori Tatarinowii Rhizoma）and Common Counterfeits Based on Ultra-High Performance Liquid Chromatography[J]. Chinese Archives of Traditional Chinese Medicine, 2025 , 43 (12) : 162 -167 . DOI: 10.13193/j.issn.1673-7717.2025.12.029
正文
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石菖蒲来源于天南星科植物石菖蒲Acorus tatarinowii Schott的干燥根茎，自1963年起被历版《中华人民共和国药典》收载至今。味辛、苦，性温。归心、胃经。具有开窍豁痰、醒神益智、化湿开胃功效，可用于治疗神昏癫痫、健忘失眠、耳鸣耳聋、脘痞不饥、噤口下痢等病症[1]。现代研究认为石菖蒲具有广泛的药理作用，包括保护神经细胞、减轻学习和记忆障碍[2-3]，调节神经递质及受体、调控凋亡因子[4-5]，抗缺血、抗心肌缺血、抗心律失常[6]、抗肿瘤[7]、抗菌和抗氧化活性等[8]。目前，石菖蒲广泛应用于中枢神经系统、心血管系统、胃肠消化系统、呼吸系统，并可用于治疗癫痫、抑郁症、失忆症、意识障碍、焦虑、失眠、失语、耳鸣、癌症、痴呆、中风、皮肤病等复杂疾病[3，9]。汉代《神农本草经》最早将菖蒲作为药材收载其中，但由于时代久远、种类繁多、分布区域广泛、早期记载不全面等原因，导致历史上石菖蒲存在名称混乱、基原偏差、功效描述杂糅混乱等现象[10]。石菖蒲与伪品来源、性状[11]、化学成分不相同[12]，药理活性[13-14]也各有侧重，故不可将伪品混用，或以伪品替代石菖蒲使用。虽然2020版《中华人民共和国药典》已对石菖蒲基原做了唯一规定，但在长期的实际应用中，市场上出现水菖蒲（又称藏菖蒲）Acorus calamus L.、茴香菖蒲（又称金钱菖蒲）Acorus gramineus Soland、九节菖蒲Anemone altaica Fisch、岩白菜Bergenia purpurascens（Hook.f.et Thoms.）Engl.等伪品作为石菖蒲销售使用的情况[15-17]。
在石菖蒲鉴别与检测方法发展过程中，先后经历过早期对其进行简单的形状、气味、颜色等性状鉴别、显微鉴别、理化、光谱鉴别[11，18-21]，再到近期的色谱-质谱联用分析[12，22]、脱氧核糖核酸（DNA）分子鉴定[23-25]等，其鉴别方法逐渐丰富和多样化，鉴别效果也得到了一定提升，但仍存在一些需要解决的问题，如石菖蒲伪品种类较多，虽然对石菖蒲真伪鉴别研究起步较早，但性状鉴别、显微和理化鉴别等传统检测方法不能准确地区分伪品，液质/气质联用以及DNA分子鉴定等鉴别方法虽能更准确，但不能同时鉴别市场上的多种伪品[26]，且不够方便快捷。
液相色谱是目前最常用的分析手段之一，液相色谱仪在各大实验室配备相对充分，本文采用超高效液相色谱（UPLC）技术建立石菖蒲真伪鉴别的有效方法，以期为进一步提升和完善石菖蒲质量控制标准、保障石菖蒲临床用药安全提供参考，并为石菖蒲真伪品鉴别的后续研究工作奠定基础。
1　仪器与材料
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1.1　仪器
ME204E型万分之一分析天平和XPR36型百万分之一分析天平由瑞士梅特勒-托利多公司提供；TC-15套式恒温器产自海宁新华；RE-3000型旋转蒸发仪由上海亚荣生化仪器提供；Waters H-class型超高效液相色谱仪由美国Waters公司提供。
1.2　材料
实验用β-细辛醚对照品（批号：112018-201601，中国食品药品检定研究院）；甲醇和乙腈（HPLC，默克公司）；磷酸和甲酸（HPLC，天津市科密欧化学试剂有限公司）；冰醋酸（HPLC，西陇科学）；石油醚60～90℃（AR，天津市永大化学试剂有限公司）；水为超纯水；其余试剂均为分析纯。实验用石菖蒲药材经广东一方制药有限公司夏天睿副高级主任药师鉴定为石菖蒲Acorus tatarinowii Schott，伪品鉴定为茴香菖蒲Acorus gramineus Soland、水菖蒲Acorus calamus L.、九节菖蒲Anemone altaica Fisch、岩白菜Bergenia purpurascens（Hook.f.et Thoms.）Engl.，来源信息见表1。
2　方法与结果
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2.1　对照品溶液的制备
取适量对照品β-细辛醚，精密称定，以甲醇为溶剂，制成每1 mL含有β-细辛醚50μg的对照品溶液，以便构建特征图谱。
2.2　供试品溶液的制备
分别精密称定石菖蒲与伪品药材粉末（过3号筛）约1 g，置于具塞锥形瓶中，再加水20 mL，并将锥形瓶置于电热套中加热回流60 min，待放冷后，以4000 r/min的速率离心10 min，取上清液，置分液漏斗中，用石油醚萃取3次，每次20 mL，合并石油醚溶液，减压回收溶液至干，残渣加70%甲醇使溶解，转移至5 mL量瓶中，加70%甲醇至刻度，摇匀，滤过，取续滤液，即得。
2.3　色谱条件
使用Waters CORTECST3（150 mm×2.1 mm，1.6μm）色谱柱；以甲醇∶乙腈＝1∶1作为流动相A，以水作为流动相B，进行梯度洗脱（0～5 min，10% ～34%A；5～13 min，34% ～35%A；13～13.5min，35%～50%A；13.5～20min，50%～62%A；20～25 min，62% ～90%A；25～26 min，90% ～10%A；26～30 min，10%～10%A）；流速为0.2 mL/min；柱温为40℃；检测波长为275 nm；进样量3μL。
2.4　方法学考察
2.4.1　专属性与参比峰选择
分别取70%甲醇空白溶剂、β-细辛醚对照品溶液以及石菖蒲供试品溶液，按照“2.3”项下色谱条件进样检测，检测得到色谱图见图1，3号峰为β-细辛醚，选定为参照峰S。专属性结果见表2，专属性考察表明各峰之间分离良好，无溶剂干扰。
2.4.2　精密度
实验人员1精密称取石菖蒲供试品一份，按“2.2”项下方法制备供试品溶液，按“2.3”项下色谱条件重复进样6次，计算得到β-细辛醚峰面积的RSD为0.82%，选定其作为参照峰（S），计算得到各共有峰的相对保留时间RSD为0.01%～0.08%、相对峰面积RSD为0.06% ～0.27%，表明仪器精密度良好。
2.4.3　重复性
精密称取同一批石菖蒲供试品6份，按“2.2”项下方法制备供试品溶液，并按“2.3”项下色谱条件进样测定，计算得到参照峰β-细辛醚峰面积的RSD为0.82%，各共有峰的相对保留时间RSD为0.01% ～0.10%、相对峰面积RSD为0.71%～2.79%，表明方法的重复性良好。
2.4.4　中间精密度
实验人员2精密称取石菖蒲供试品一份，按“2.2”项下方法制备供试品溶液，按“2.3”项下色谱条件在另一台同型号仪器重复进样6次，计算2.4.2项下实验人员1所测得参照峰β-细辛醚峰面积与实验人员2所测得β-细辛醚峰面积的RSD为1.93%，计算得到各共有峰的相对保留时间RSD为0.02%～1.23%、相对峰面积的RSD为1.74%～3.32%，表明中间精密度良好。
2.4.5　样品稳定性
分别于0、2、4、6、8、10、12、18、24 h，精密吸取石菖蒲供试品溶液按照“2.3”项下规定的色谱条件进行进样测定，计算得到参照峰β-细辛醚峰面积的RSD为0.20%，计算得到各共有峰的相对保留时间的RSD 为0.01%～0.24%、相对峰面积的RSD为0.03%～0.47%，实验结果表明本方法所制得的供试品溶液在24 h内非常稳定。
2.4.6　耐用性
（1）不同柱温、流速、进样量考察：考察不同柱温（35、40、45℃），不同流速（0.18、0.20、0.22 mL/min），不同进样量（1、2、3μL）等条件改变对该方法的影响，除改变考察条件外，按照“2.3”项下色谱条件进样测定，以β细辛醚为参照峰（S），计算得到在不同柱温、流速、进样量条件下，各共有峰的相对保留时间RSD分别为0.01% ～1.39%、0.01% ～3.34%、0.03%～0.14%；各共有峰的相对峰面积RSD分别为0.17%～2.43%、0.48%～2.09%、0.25% ～1.28%；表明此法耐用性较好，可在条件微小变动情况下稳定出峰。（2）不同色谱柱考察：本实验对3根同型号Waters CORTECS T3（2.1 mm ×150 mm，1.6μm）色谱柱进行考察，按照“2.3”项下色谱条件进样测定，计算得到参照峰β-细辛醚峰面积的RSD为0.87%，计算得到各共有峰的相对保留时间RSD 为0.01%～0.21%、各共有峰的相对峰面积的RSD为0.19% ～0.62%，实验结果表明色谱柱耐用性良好。
2.5　样品检测
分别取20批石菖蒲、4批茴香菖蒲、3批水菖蒲、4批九节菖蒲、3批岩白菜，按“2.2”项下方法制备样品溶液，按“2.3”项下色谱条件进样测定并记录色谱图，色谱图数据导入“中药色谱指纹图谱相似度评价系统（2012版）”生成对照图谱，结果见插页ⅩⅩⅨ图2-图4、插页ⅩⅩⅩ图5-图6；石菖蒲与伪品谱图对比见图7。石菖蒲药材确定4个共有峰，茴香菖蒲和水菖蒲各确定6个共有峰，九节菖蒲和岩白菜各确定1个共有峰。其中，5、6号色谱峰为茴香菖蒲的特征峰，7、8号色谱峰为水菖蒲的特征峰，9号色谱峰为九节菖蒲和岩白菜的特征峰，此法可作为石菖蒲药材与伪品鉴别的有效方法。通过与对照品比对，指认了3号色谱峰为β-细辛醚，并以其作为参照峰S，所有批次石菖蒲及伪品的各共有峰保留时间或相对保留时间RSD均小于0.5%，各共有峰峰面积或相对峰面积结果见表3-表6。相似度评价结果见表7。石菖蒲样品特征图谱相似度在0.892～0.996，伪品样品各自的特征图谱相似度在0.938以上。
3　讨论
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3.1　供试品溶液制备方法的考察
分别考察了不同加水量、不同煎煮时间、不同萃取次数、不同萃取体积、不同浓度甲醇作为复溶溶剂等条件，进行供试品溶液制备，进样检测并进行数据分析，数据结果见表8。最终结合“总峰面积与称样量比值”及“峰3面积百分比”选择制样条件，因石菖蒲中主要成分是峰3（β-细辛醚），考虑到色谱图呈现的稳定性、直观性，应选择总峰面积与称样量比值较大、峰3面积百分比较小的制样条件，综合能源、时间成本、经济效益等因素，确定最终样品制备条件见“2.2”项下供试品溶液的制备。当以萃取溶剂石油醚对石菖蒲水煎液进行萃取时，每次萃取量为20 mL石油醚较适宜，而当石油醚体积为10 mL时，进行轻微的振荡即产生严重乳化现象，需要进行长时间加热才能使乳化分层，体积为20 mL石油醚萃取水煎液时体积比近似1∶1，既不会轻易乳化，也能使两相更充分接触，因此萃取体积确定为20 mL。
3.2　超高效液相色谱流动相条件考察
3.2.1　流动相A的考察
以十八烷基硅烷键合硅胶为填充剂（柱长为150 mm，内径为2.1 mm，粒径为1.6μm）；以不同的有机溶剂为流动相A，以水为流动相B，其余条件按2.3项下规定分别进行梯度洗脱；流动相A的种类包括：纯甲醇、甲醇∶乙腈＝3∶1、甲醇∶乙腈＝2∶1、甲醇∶乙腈＝1∶1、甲醇∶乙腈＝1∶2、甲醇∶乙腈＝1∶3、纯乙腈。
不同种类流动相A的色谱检测的对比结果如图8，根据图8，甲醇比例越高，峰3与峰4分离度越大，但是甲醇的比例过高，导致峰2的峰型变差，因此，选择甲醇∶乙腈＝1∶1为流动相A，峰2峰型较好且出峰较稳定。
3.2.2　流动相B的考察
以十八烷基硅烷键合硅胶为填充剂（柱长为150 mm，内径为2.1 mm，粒径为1.6μm）；以甲醇∶乙腈＝1∶1为流动相A，以不同的水溶液为流动相B，其余条件按2.3项下规定分别进行梯度洗脱；流动相B的种类包括0.1%磷酸、0.1%甲酸、0.1%冰醋酸、超纯水。
不同种类流动相B的色谱检测的对比结果如图9，根据图9，流动相B的种类对特征图谱影响不大，从成本节省和便于操作的角度考虑，选择超纯水作为水相。
3.3　特征图谱测定结果讨论
本方法建立的石菖蒲真伪鉴别特征图谱可以快速便捷区分石菖蒲与伪品茴香菖蒲、水菖蒲、九节菖蒲及岩白菜，本法建立的20批石菖蒲样品特征图谱相似度在0.892以上，不同批次之间共有峰峰面积存在差异，石菖蒲的主要有效成分是挥发油类，容易在加工干燥过程中造成不同程度损失，因此共有峰之间差异可能是石菖蒲不同产地、加工保存方式不同等因素导致的。
综上，本实验建立的石菖蒲真伪鉴别特征图谱方法简便、快速、稳定，可用于石菖蒲与常见伪品茴香菖蒲、水菖蒲、九节菖蒲及岩白菜的区分，对于控制石菖蒲药材的质量具有一定的参考意义。
基金
收起
  • 国家工信部产业技术基础公共服务平台项目(2022-230-221)
  • 佛山市南海区重点领域科技攻关专项(南科〔2023〕20号-18)
文献
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2025年第43卷第12期
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doi: 10.13193/j.issn.1673-7717.2025.12.029
  • 首发时间：2026-04-29
  • 出版时间：2025-12-10
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基金
国家工信部产业技术基础公共服务平台项目(2022-230-221)
佛山市南海区重点领域科技攻关专项(南科〔2023〕20号-18)
作者信息
    1.南方医科大学中医药学院，广东省中药制剂重点实验室，广东 广州 510515
    2.广东一方制药有限公司，广东省中药配方颗粒企业重点实验室，广东 佛山 528244

通讯作者:

谭晓梅（1963-），女，湖南澧县人，研究员，博士研究生导师，博士，研究方向：中药新制剂及中药复方配伍规律。Email：。
陈向东（1975-），男，广东梅州人，教授，硕士研究生导师，硕士，研究方向：中药饮片及中药配方颗粒。E-mail：。
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2种不同金属材料的力学参数
科
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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