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Article(id=1193476458191487099, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1193476452629836735, articleNumber=1001-2494(2025)04-0334-15, orderNo=null, doi=10.11669/cpj.2025.04.004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1721750400000, receivedDateStr=2024-07-24, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1762476561352, onlineDateStr=2025-11-07, pubDate=1740153600000, pubDateStr=2025-02-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1762476561352, onlineIssueDateStr=2025-11-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1762476561352, creator=13701087609, updateTime=1762476561352, updator=13701087609, issue=Issue{id=1193476452629836735, tenantId=1146029695717560320, journalId=1190317699101192196, year='2025', volume='60', issue='4', pageStart='313', pageEnd='438', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1762476560027, creator=13701087609, updateTime=1762482957432, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1193503285370913518, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1193476452629836735, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1193503285370913519, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1193476452629836735, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=334, endPage=348, ext={EN=ArticleExt(id=1193476459986649218, articleId=1193476458191487099, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Research on the Identification Characteristics of Synthetic and Natural Cinnabar Based on Multispectral Analyses, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To investigate crystal structure and composition of synthetic and natural cinnaba,compare their spectroscopic characteristics and analyze their microscopic characteristics and trace element differences. METHODS This investigation endeavors to clarify the crystal configuration and phase composition of synthetic and natural cinnabar on the market and analyze the differences in trace elements between them. Meanwhile, we used powder X-ray diffraction, Raman spectroscopy, attenuated total reflection-Fourier transform infrared spectroscopy, electron probe micro-analysis, inductively coupled plasma mass spectrometry, with traditional microscopic identification(characteristics; optical polarized light microscopy), to explore the identification methods of synthetic and natural cinnabar. RESULTS The results suggest that, both present to share the same characteristics in the crystal forms of synthetic and natural cinnabar. Common impurities in natural cinnabar are quartz, pyrite, calcite, stibnite, etc., while the differences among different batches of samples are distinguishable. Synthetic cinnabar contains a small number of calcite impurities, and the quality is relatively uniform. By using electron probe micro-analysis technology, and powder crystal X-ray diffraction technology combined with polarized light microscopy, the impurities in synthetic cinnabar and natural cinnabar can be effectively analyzed and identified; the mid-infrared spectrum and Raman spectrum characteristics of synthetic and natural cinnabar are similar; the characteristic trace elements between synthetic and natural cinnabar are consistent. CONCLUSION Three elements including Fe, Mg and Zn can be quantified to identify these two as reference.

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目的 研究合成朱砂和天然朱砂的晶体构型和物相组成,对比合成朱砂和天然朱砂光谱学特征,分析其显微特征及微量元素差异。方法 采用粉晶X射线衍射、拉曼光谱、傅里叶红外光谱、电子探针微区分析、电感耦合等离子体质谱等方法,探索合成朱砂和天然朱砂的鉴别方法。结果 研究表明合成朱砂和天然朱砂的晶型相同;天然朱砂中常见的杂质为石英、黄铁矿、方解石、辉锑矿等;合成朱砂中含有极少量的方解石杂质,质量较为均一;通过使用电子探针微区分析技术或粉晶X射线衍射技术结合偏光显微法,可有效对合成朱砂和天然朱砂中的杂质进行分析。结论 合成朱砂和天然朱砂的中红外光谱和拉曼光谱特征相似,其特征微量元素一致,通过等离子体电感耦合质谱法,可将铁、镁、锌3种元素作为二者鉴别的参考。

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*骆璐,女,博士,助理研究员 研究方向:中药质量控制
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魏梦佳,女,硕士研究生 研究方向:中药质量控制

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魏梦佳,女,硕士研究生 研究方向:中药质量控制

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魏梦佳,女,硕士研究生 研究方向:中药质量控制

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The botanical origins and sources of cinnabar[J]. 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J Chengdu Univ Tradit Chin Med(成都中医药大学学报), 1982, 1:59., articleTitle=Cinnabar and its synthesis, refAbstract=null), Reference(id=1193540679163932950, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, doi=null, pmid=null, pmcid=null, year=1993, volume=null, issue=null, pageStart=103, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=6, authorNames=TANG S W, journalName=Reconstruct The Political And Historical Evidence Class Spare Materia Medica(重修政和经史证类备用本草), refType=null, unstructuredReference=TANG S W. Reconstruct The Political And Historical Evidence Class Spare Materia Medica(重修政和经史证类备用本草)[M]. Beijing: Huaxia Publishing House, 1993:103., articleTitle=null, refAbstract=null), Reference(id=1193540679247819031, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, doi=null, pmid=null, pmcid=null, year=1991, volume=null, issue=null, pageStart=1222, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=7, authorNames=ZHANG J B, journalName=Jing Yue Quanshu(景岳全书), refType=null, unstructuredReference=ZHANG J B. Jing Yue Quanshu(景岳全书)[M]. Beijing: People's Medical Publishing House, 1991:1222., articleTitle=null, refAbstract=null), Reference(id=1193540679302344984, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, doi=null, pmid=null, pmcid=null, year=1959, volume=null, issue=null, pageStart=11, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=8, authorNames=ZHANG L, journalName=This Scripture is the Original(本经逢原), refType=null, unstructuredReference=ZHANG L. This Scripture is the Original(本经逢原)[M]. Shanghai: Shanghai Science and Technology Press, 1959:11-12., articleTitle=null, refAbstract=null), Reference(id=1193540679365259545, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, doi=null, pmid=null, pmcid=null, year=2023, volume=58, issue=21, pageStart=1922, pageEnd=1930, url=null, language=null, rfNumber=[10], rfOrder=9, authorNames=ZHUO Y Z, LIU X X, WANG X S, journalName=Chin Pharm J(中国药学杂志), refType=null, unstructuredReference=ZHUO Y Z, LIU X X, WANG X S, et al. Study on the microstructure and differences of major and trace element contents of cinnabar and its different processed products[J]. Chin Pharm J(中国药学杂志), 2023, 58(21):1922-1930., articleTitle=Study on the microstructure and differences of major and trace element contents of cinnabar and its different processed products, refAbstract=null), Reference(id=1193540679423979802, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, doi=null, pmid=null, pmcid=null, year=2018, volume=34, issue=5, pageStart=165, pageEnd=167, url=null, language=null, rfNumber=[11], rfOrder=10, authorNames=YANG H G, LI L, WANG Y H, journalName=Pharm Clin Chin Mater Med, refType=null, unstructuredReference=YANG H G, LI L, WANG Y H, et al. Historical understanding and evaluation of cinnabar poison in traditional Chinese medicine[J]. 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A-cinnabar(A1-A25); B-Calcite(B1-B25); C-white and transparent impurity(C1-C25).

, figureFileSmall=J8ZKA6jOTAlFw5Dyj+TwnQ==, figureFileBig=t9gnB/mxYHfPGReoV+Zlzg==, tableContent=null), ArticleFig(id=1193540676764791029, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图2, caption=合成朱砂粉末正交偏光显微特征(标尺=50 μm)

A-朱砂晶体(A1~A25);B-方解石(B1~B25); C-白色透明杂质(C1~C25)。

, figureFileSmall=J8ZKA6jOTAlFw5Dyj+TwnQ==, figureFileBig=t9gnB/mxYHfPGReoV+Zlzg==, tableContent=null), ArticleFig(id=1193540676819316982, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.3, caption=Orthogonal polarization microscopic characteristics of natural cinnabar powder(scale=50 μm)

A-cinnabar and calcite(A1-A19); B-white and transparent impurity(B1-B15).

, figureFileSmall=cbdNvxR+HtdM3cHmr5a3ag==, figureFileBig=f+2AhRDFX/L+gLeCysitbg==, tableContent=null), ArticleFig(id=1193540676890620151, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图3, caption=天然朱砂粉末正交偏光显微特征(标尺=50 μm)

A-朱砂晶体和方解石(A1~A19); B-白色透明杂质(B1~B15)。

, figureFileSmall=cbdNvxR+HtdM3cHmr5a3ag==, figureFileBig=f+2AhRDFX/L+gLeCysitbg==, tableContent=null), ArticleFig(id=1193540676970311928, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.4, caption=Orthogonal polarization microscopic characteristics of the thin-selection of synthetic cinnabar(scale=100 μm)

A-reflection(A1-A25); B-transmission(B1-B25).

, figureFileSmall=eyar/eCyWTI1T6Dr8Disfg==, figureFileBig=VWzDTstZ7BCi/ZDs7juOQQ==, tableContent=null), ArticleFig(id=1193540677050003705, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图4, caption=合成朱砂薄片正交偏光显微特征(标尺=100 μm)

A-反射(A1~A25); B-透射(B1~B25)。

, figureFileSmall=eyar/eCyWTI1T6Dr8Disfg==, figureFileBig=VWzDTstZ7BCi/ZDs7juOQQ==, tableContent=null), ArticleFig(id=1193540677138084090, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.5, caption=Orthogonal polarization microscopic characteristics of the thin-selection of natural cinnabar(scale=100 μm)

A-reflection(A1-A19); B-C-transmission(B1-B19,C1-C19).

, figureFileSmall=Am9CBHQ8Sw5/Xcu6hWFJtw==, figureFileBig=wnyYx+B+fIEGPbvrND1SdA==, tableContent=null), ArticleFig(id=1193540677238747387, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图5, caption=天然朱砂薄片正交偏光显微特征(标尺=100 μm)

A-反射(A1~A19);B~C-透射(B1~B19,C1~C19)。

, figureFileSmall=Am9CBHQ8Sw5/Xcu6hWFJtw==, figureFileBig=wnyYx+B+fIEGPbvrND1SdA==, tableContent=null), ArticleFig(id=1193540677297467644, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.6, caption=Fourier transform infrared spectrum and Raman spectral characteristics of natural and synthetic cinnabar

A-infrared spectrum of synthetic cinnabar(S1-S25); B-infrared spectrum of natural cinnabar(N1-N19); C-Raman spectral characteristics of synthetic cinnabar(S1-S25); D-Raman spectral characteristics of natural cinnabar(N1-N19).

, figureFileSmall=hQoL3SczvMpKdA7IzuvTxA==, figureFileBig=bf9xROEKyETWyk59eZQMvg==, tableContent=null), ArticleFig(id=1193540677356187901, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图6, caption=天然与合成朱砂的红外及拉曼光谱

A-合成朱砂红外光谱(S1~S25);B-天然朱砂的红外光谱(N1~N19);C-合成朱砂拉曼光谱(S1~S25);D-天然朱砂拉曼光谱(N1~N19)。

, figureFileSmall=hQoL3SczvMpKdA7IzuvTxA==, figureFileBig=bf9xROEKyETWyk59eZQMvg==, tableContent=null), ArticleFig(id=1193540677444268286, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.7, caption=Average intensity between each Raman spectrum sample of synthetic and natural cinnabar

A-average intensity between each Raman spectrum sample of synthetic cinnabar; B-average intensity correlation diagram of synthetic and natural cinnabar; C-average intensity between each Raman spectrum sample of natural cinnabar; D-average intensity bar graph of synthetic and natural cinnabar.

, figureFileSmall=iTzgk57pUoP7uUeRsVtU2w==, figureFileBig=D+gzB0u54RxCdYrzRSlU4g==, tableContent=null), ArticleFig(id=1193540677519765759, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图7, caption=合成朱砂和天然朱砂每个拉曼光谱样本之间的平均强度

A-合成朱砂每个拉曼光谱样本之间的平均强度; B-合成朱砂和天然朱砂的平均强度相关图; C-天然朱砂每个拉曼光谱样本之间的平均强度; D-合成朱砂和天然朱砂的平均强度柱状图。

, figureFileSmall=iTzgk57pUoP7uUeRsVtU2w==, figureFileBig=D+gzB0u54RxCdYrzRSlU4g==, tableContent=null), ArticleFig(id=1193540677591068928, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.8, caption=Comparison of X-ray patterns between synthetic and natural cinnabar

A-X-ray of syntheticcinnabar(S1-S25); B-X-ray of natural cinnabar(N1-N19).

, figureFileSmall=XSVDw4AM1XOu6nS/u15pVA==, figureFileBig=jLvlnxi0xulJTfYHAUdh/g==, tableContent=null), ArticleFig(id=1193540677649789185, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图8, caption=合成和天然朱砂X射线衍射图谱

A-合成朱砂X射线衍射图谱(S1~S25);B-天然朱砂X射线衍射图谱(N1~N19)。

, figureFileSmall=XSVDw4AM1XOu6nS/u15pVA==, figureFileBig=jLvlnxi0xulJTfYHAUdh/g==, tableContent=null), ArticleFig(id=1193540677712703746, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.9, caption=Backscattered electron image of synthetic cinnabar

A-backscattered electron image of synthetic cinnabar S1; B-backscattered electron image of synthetic cinnabar S4; C-backscattered electron image of synthetic cinnabar S5; D-backscattered electron image of synthetic cinnabar S7; E-backscattered electron image of synthetic cinnabar S15; F-backscattered electron image of synthetic cinnabar S18.

, figureFileSmall=XtqbVQoR2QbPVPhHYMohBg==, figureFileBig=ehedvwm0pPHewL4mAliLcA==, tableContent=null), ArticleFig(id=1193540677771424003, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图9, caption=合成朱砂背散射电子图

A-合成朱砂S1背散射电子图;B-合成朱砂S4背散射电子图;C-合成朱砂S5背散射电子图;D-合成朱砂S7背散射电子图;E-合成朱砂S15背散射电子图;F-合成朱砂S18背散射电子图。

, figureFileSmall=XtqbVQoR2QbPVPhHYMohBg==, figureFileBig=ehedvwm0pPHewL4mAliLcA==, tableContent=null), ArticleFig(id=1193540677830144260, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.10, caption=Backscattered electron image of natural cinnabar

A-B-backscattered electron images of natural cinnabar N1; C-D-backscattered electron images of natural cinnabar N3; E-F-backscattered electron images of natural cinnabar N5; G-H-backscattered electron images of natural cinnabar N9.

, figureFileSmall=Uo4azJe8nAxQzdsyEAZDcw==, figureFileBig=nSoaPBkVhEtf5v0+WNyyBA==, tableContent=null), ArticleFig(id=1193540677888864517, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图10, caption=天然朱砂背散射电子图

A~B-天然朱砂N1背散射电子图;C~D-天然朱砂N3背散射电子图;E~F-天然朱砂N5背散射电子图;G~H-天然朱砂N9背散射电子图。

, figureFileSmall=Uo4azJe8nAxQzdsyEAZDcw==, figureFileBig=nSoaPBkVhEtf5v0+WNyyBA==, tableContent=null), ArticleFig(id=1193540677947584774, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Fig.11, caption=Comparative analysis of the average content of trace elements in synthetic and natural cinnabar

A-line chart comparing the average content of trace elements in synthetic and natural cinnabar; B-dot-line chart comparing the average content of trace elements in synthetic and natural cinnabar; C-average intensity of trace elements in synthetic cinnabar; D-average intensity of trace elements in natural cinnabar; E-average content of trace elements; F-P value of trace element t test; G-measured values of each group of elements with 10 minimum P values.

, figureFileSmall=mPqPJR+PYHPpsHhnCgncCw==, figureFileBig=PISb7YG9V+efV21+0zpeaw==, tableContent=null), ArticleFig(id=1193540678002110727, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=图11, caption=合成和天然朱砂微量元素平均含量比较分析

A-合成和天然朱砂微量元素平均含量比较折线图;B-合成和天然朱砂微量元素平均含量比较点线图;C-合成朱砂微量元素平均强度;D-天然朱砂微量元素平均强度;E-微量元素平均含量;F-微量元素t检测P值;G-10个最小P值的每组元素的测量值。

, figureFileSmall=mPqPJR+PYHPpsHhnCgncCw==, figureFileBig=PISb7YG9V+efV21+0zpeaw==, tableContent=null), ArticleFig(id=1193540678056636680, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Tab.1, caption=

Information of synthetic and natural cinnabar samples

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Batch No. Sample Name Origin(in Chinese) No. Batch No. Sample Name Origin(in Chinese)
S1 2022052701 Synthetic cinnabar Anguo,Hebei province(河北安国) S23 2022061323 Synthetic cinnabar Baozhou,Anhui province(安徽亳州)
S2 2022060102 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) S24 2022061324 Synthetic cinnabar Bozhou,Anhui province(安徽亳州)
S3 2022060203 Synthetic cinnabar Lotus pond,Sichuan province(四川荷花池) S25 2022061325 Synthetic cinnabar Bozhou,Anhui province(安徽亳州)
S4 2022060204 Synthetic cinnabar Lotus pond,Sichuan province(四川荷花池) N1 2022061501 Natural cinnabar Beijing(北京)
S5 2022060305 Synthetic cinnabar Xiangxi,Hunan province(湖南湘西) N2 2022061502 Natural cinnabar Hunan provience(湖南)
S6 2022060406 Synthetic cinnabar Bozhou City,Anhui province(安徽亳州) N3 2022061503 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S7 2022060607 Synthetic cinnabar Bozhou City,Anhui province(安徽亳州) N4 2022061504 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S8 2022060608 Synthetic cinnabar Tongren,Guizhou province(贵州铜仁) N5 2022061505 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S9 2022061109 Synthetic cinnabar Xiangxi,Hunan province(湖南湘西) N6 2022061506 Natural cinnabar Anguo,Hebei province(河北安国)
S10 2022061110 Synthetic cinnabar Jinhua,Zhejiang province(浙江金华) N7 2022052707 Natural cinnabar Anguo,Hebei province(河北安国)
S11 2022061111 Synthetic cinnabar Jinhua,Zhejiang province(浙江金华) N8 2022050808 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S12 2022061112 Synthetic cinnabar Lianyungang,Jiangsu province(江苏连云港) N9 2022052809 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S13 2022061113 Synthetic cinnabar Zhengzhou,Henan province(河南郑州) N10 2022052810 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S14 2022061114 Synthetic cinnabar Lianyungang,Jiangsu province(江苏连云港) N11 2022060111 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S15 2022061215 Synthetic cinnabar Shangqiu,Henan province(江苏宿迁) N12 2022060612 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S16 2022061216 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) N13 2022060713 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S17 2022061217 Synthetic cinnabar Suqian,Jiangsu province(江苏宿迁) N14 2022060814 Natural cinnabar Suqian,Jiangsu province(江苏宿迁)
S18 2022061218 Synthetic cinnabar Jining,Shandong province(山东济宁) N15 2022060915 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S19 2022061219 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) N16 2022061116 Natural cinnabar Lianyungang,Jiangsu province(江苏连云港)
S20 2022061320 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) N17 2022061117 Natural cinnabar Chengdu,Sichuan province(四川成都)
S21 2022052821 Synthetic cinnabar Lotus pond,Sichuan province(四川荷花池) N18 2022061218 Natural cinnabar Tongren,Guizhou province(贵州铜仁)
S22 2022061122 Synthetic cinnabar Xuchang,Henan province(河南许昌) N19 2022061309 Natural cinnabar Shenzhen,Guangdong province(广东深圳)
), ArticleFig(id=1193540678127939849, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=表1, caption=

合成和天然朱砂样品信息

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Batch No. Sample Name Origin(in Chinese) No. Batch No. Sample Name Origin(in Chinese)
S1 2022052701 Synthetic cinnabar Anguo,Hebei province(河北安国) S23 2022061323 Synthetic cinnabar Baozhou,Anhui province(安徽亳州)
S2 2022060102 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) S24 2022061324 Synthetic cinnabar Bozhou,Anhui province(安徽亳州)
S3 2022060203 Synthetic cinnabar Lotus pond,Sichuan province(四川荷花池) S25 2022061325 Synthetic cinnabar Bozhou,Anhui province(安徽亳州)
S4 2022060204 Synthetic cinnabar Lotus pond,Sichuan province(四川荷花池) N1 2022061501 Natural cinnabar Beijing(北京)
S5 2022060305 Synthetic cinnabar Xiangxi,Hunan province(湖南湘西) N2 2022061502 Natural cinnabar Hunan provience(湖南)
S6 2022060406 Synthetic cinnabar Bozhou City,Anhui province(安徽亳州) N3 2022061503 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S7 2022060607 Synthetic cinnabar Bozhou City,Anhui province(安徽亳州) N4 2022061504 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S8 2022060608 Synthetic cinnabar Tongren,Guizhou province(贵州铜仁) N5 2022061505 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S9 2022061109 Synthetic cinnabar Xiangxi,Hunan province(湖南湘西) N6 2022061506 Natural cinnabar Anguo,Hebei province(河北安国)
S10 2022061110 Synthetic cinnabar Jinhua,Zhejiang province(浙江金华) N7 2022052707 Natural cinnabar Anguo,Hebei province(河北安国)
S11 2022061111 Synthetic cinnabar Jinhua,Zhejiang province(浙江金华) N8 2022050808 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S12 2022061112 Synthetic cinnabar Lianyungang,Jiangsu province(江苏连云港) N9 2022052809 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S13 2022061113 Synthetic cinnabar Zhengzhou,Henan province(河南郑州) N10 2022052810 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S14 2022061114 Synthetic cinnabar Lianyungang,Jiangsu province(江苏连云港) N11 2022060111 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S15 2022061215 Synthetic cinnabar Shangqiu,Henan province(江苏宿迁) N12 2022060612 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S16 2022061216 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) N13 2022060713 Natural cinnabar Bozhou,Anhui province(安徽亳州)
S17 2022061217 Synthetic cinnabar Suqian,Jiangsu province(江苏宿迁) N14 2022060814 Natural cinnabar Suqian,Jiangsu province(江苏宿迁)
S18 2022061218 Synthetic cinnabar Jining,Shandong province(山东济宁) N15 2022060915 Natural cinnabar Lotus pond,Sichuan province(四川荷花池)
S19 2022061219 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) N16 2022061116 Natural cinnabar Lianyungang,Jiangsu province(江苏连云港)
S20 2022061320 Synthetic cinnabar Bozhou,Anhui province(安徽亳州) N17 2022061117 Natural cinnabar Chengdu,Sichuan province(四川成都)
S21 2022052821 Synthetic cinnabar Lotus pond,Sichuan province(四川荷花池) N18 2022061218 Natural cinnabar Tongren,Guizhou province(贵州铜仁)
S22 2022061122 Synthetic cinnabar Xuchang,Henan province(河南许昌) N19 2022061309 Natural cinnabar Shenzhen,Guangdong province(广东深圳)
), ArticleFig(id=1193540678190854410, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Tab.2, caption=

Search and match results,grain size and microscopic stress of synthetic and natural cinnabar

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Sample
name		 PDF standard card XS(A)
/Å		 Strain
/%
Phase Chemical formula PDF-# Space group
S1 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 475 0.115
S2 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 2 470 0.155
S3 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 956 0.082
S4 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 491 0.130
S5 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 402 0.124
S6 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 495 0.111
S7 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 403 0.128
S8 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 2 112 0.141
S9 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 336 0.107
S10 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 037 0.094
S11 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 632 0.149
S12 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 679 0.068
S13 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 815 0.120
S14 Synthetic cinnabar Cinnabar,syn HgS 80-2192 P3221(154) 1 144 0.095
S15 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 447 0.113
S16 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 651 0.117
S17 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 480 0.120
S18 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 736 0.121
S19 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 887 0.145
S20 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 440 0.110
S21 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 313 0.130
S22 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 961 0.105
S23 Synthetic cinnabar Cinnabar, syn HgS 80-2192 P3221(154) 1 460 0.143
S24 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 109 0.115
S25 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 487 0.140
N1 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 3 751 0.131
N2 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 636 0.015
N3 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 057 0.071
N4 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 218 0.089
N5 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 158 0.066
N6 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 089 0.068
N7 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 996 0.085
N8 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 962 0.070
N9 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 444 0.093
N10 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 830 0.109
N11 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 632 0.058
N12 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 839 0.114
N13 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 988 0.053
N14 Natural cinnabar Mercury sulfide, HP HgS 89-0438 P3121(152) 887 0.095
N15 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 583 0.014
N16 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 004 0.066
N17 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 098 0.100
N18 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 315 0.087
N19 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 059 0.073
), ArticleFig(id=1193540678266351883, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=表2, caption=

合成和天然朱砂物相检索结果、晶粒尺寸及微观应力数据

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Sample
name		 PDF standard card XS(A)
/Å		 Strain
/%
Phase Chemical formula PDF-# Space group
S1 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 475 0.115
S2 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 2 470 0.155
S3 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 956 0.082
S4 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 491 0.130
S5 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 402 0.124
S6 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 495 0.111
S7 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 403 0.128
S8 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 2 112 0.141
S9 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 336 0.107
S10 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 037 0.094
S11 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 632 0.149
S12 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 679 0.068
S13 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 815 0.120
S14 Synthetic cinnabar Cinnabar,syn HgS 80-2192 P3221(154) 1 144 0.095
S15 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 447 0.113
S16 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 651 0.117
S17 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 480 0.120
S18 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 736 0.121
S19 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 887 0.145
S20 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 440 0.110
S21 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 313 0.130
S22 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 961 0.105
S23 Synthetic cinnabar Cinnabar, syn HgS 80-2192 P3221(154) 1 460 0.143
S24 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 109 0.115
S25 Synthetic cinnabar Cinnabar HgS 99-0031 P3121(152) 1 487 0.140
N1 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 3 751 0.131
N2 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 636 0.015
N3 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 057 0.071
N4 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 218 0.089
N5 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 158 0.066
N6 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 089 0.068
N7 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 996 0.085
N8 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 962 0.070
N9 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 444 0.093
N10 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 830 0.109
N11 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 632 0.058
N12 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 839 0.114
N13 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 988 0.053
N14 Natural cinnabar Mercury sulfide, HP HgS 89-0438 P3121(152) 887 0.095
N15 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 583 0.014
N16 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 004 0.066
N17 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 098 0.100
N18 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 315 0.087
N19 Natural cinnabar Cinnabar HgS 99-0031 P3121(152) 1 059 0.073
), ArticleFig(id=1193540678341849356, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=EN, label=Tab.3, caption=

The average content of trace elements in synthetic and natural cinnabar. μg·g-1

, figureFileSmall=null, figureFileBig=null, tableContent=
Trace
element		 The average content of
synthetic cinnabar/%		 The average content of
natural cinnabar/%		 Trace
element		 The average content of
synthetic cinnabar/%		 The average content of
natural cinnabar/%
Ag 0.36 5.04 Nb 0.18 0.22
Al 4.19 22.61 Nd 0.34 1.18
As 0.97 102.74 Ni 0.37 2.14
Au 18.87 22.77 Os 0.15 0.19
B 0.53 0.47 P 1.62 5.18
Ba 0.58 20.06 Pb 0.57 96.34
Be 0.01 0.02 Pd 0.96 0.69
Bi 0.91 1.19 Pr 0.21 0.94
Ca 50.85 2 070.07 Pt 1.55 9.84
Cd 0.11 49.51 Rb 1.95 3.19
Ce 0.38 3.13 Re 0.50 0.53
Co 0.16 1.23 Rh 0.53 48.39
Cr 0.51 9.79 Ru 0.54 0.98
Cs 0.16 1.23 Sb 3.33 3 851.57
Cu 29.55 28.13 Sc 0.22 1.85
Dy 0.08 0.15 Se 1.35 670.91
Er 0.06 0.10 Si 28.33 77.31
Eu 0.02 0.04 Sm 0.21 0.36
Fe 6.06 2 314.16 Sn 1.84 724.20
Ga 1.02 2.18 Sr 0.18 2.04
Gd 0.10 0.15 Ta 0.45 0.68
Ge 2.22 1.91 Tb 0.15 0.19
Hf 0.23 0.97 Te 2.76 22.23
Ho 0.10 0.56 Th 1.02 3.76
In 0.43 2.48 Ti 0.09 0.66
Ir 0.60 0.87 Tl 1.58 1.15
K 3.65 16.24 Tm 0.07 0.37
La 0.04 1.33 U 0.56 0.91
Li 0.08 0.11 V 0.08 0.17
Lu 0.05 0.11 W 0.62 0.78
Mg 2.43 805.04 Y 0.05 0.20
Mn 0.24 85.29 Yb 0.02 0.03
Mo 1.15 3.07 Zn 1.53 492.88
Na 10.07 23.91 Zr 0.22 0.13
), ArticleFig(id=1193540678425735437, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193476458191487099, language=CN, label=表3, caption=

合成和天然朱砂微量元素平均含量。μg·g-1

, figureFileSmall=null, figureFileBig=null, tableContent=
Trace
element		 The average content of
synthetic cinnabar/%		 The average content of
natural cinnabar/%		 Trace
element		 The average content of
synthetic cinnabar/%		 The average content of
natural cinnabar/%
Ag 0.36 5.04 Nb 0.18 0.22
Al 4.19 22.61 Nd 0.34 1.18
As 0.97 102.74 Ni 0.37 2.14
Au 18.87 22.77 Os 0.15 0.19
B 0.53 0.47 P 1.62 5.18
Ba 0.58 20.06 Pb 0.57 96.34
Be 0.01 0.02 Pd 0.96 0.69
Bi 0.91 1.19 Pr 0.21 0.94
Ca 50.85 2 070.07 Pt 1.55 9.84
Cd 0.11 49.51 Rb 1.95 3.19
Ce 0.38 3.13 Re 0.50 0.53
Co 0.16 1.23 Rh 0.53 48.39
Cr 0.51 9.79 Ru 0.54 0.98
Cs 0.16 1.23 Sb 3.33 3 851.57
Cu 29.55 28.13 Sc 0.22 1.85
Dy 0.08 0.15 Se 1.35 670.91
Er 0.06 0.10 Si 28.33 77.31
Eu 0.02 0.04 Sm 0.21 0.36
Fe 6.06 2 314.16 Sn 1.84 724.20
Ga 1.02 2.18 Sr 0.18 2.04
Gd 0.10 0.15 Ta 0.45 0.68
Ge 2.22 1.91 Tb 0.15 0.19
Hf 0.23 0.97 Te 2.76 22.23
Ho 0.10 0.56 Th 1.02 3.76
In 0.43 2.48 Ti 0.09 0.66
Ir 0.60 0.87 Tl 1.58 1.15
K 3.65 16.24 Tm 0.07 0.37
La 0.04 1.33 U 0.56 0.91
Li 0.08 0.11 V 0.08 0.17
Lu 0.05 0.11 W 0.62 0.78
Mg 2.43 805.04 Y 0.05 0.20
Mn 0.24 85.29 Yb 0.02 0.03
Mo 1.15 3.07 Zn 1.53 492.88
Na 10.07 23.91 Zr 0.22 0.13
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合成朱砂与天然朱砂的鉴别特征研究
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魏梦佳 1 , 辛雪颖 1 , 段雯雯 1 , 李娆娆 1 , 王翘楚 2 , 顾雪竹 1 , 骆璐 1, *
中国药学杂志 | 论著 2025,60(4): 334-348
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中国药学杂志 | 论著 2025, 60(4): 334-348
合成朱砂与天然朱砂的鉴别特征研究
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魏梦佳1, 辛雪颖1, 段雯雯1, 李娆娆1, 王翘楚2, 顾雪竹1, 骆璐1, *
作者信息
  • 1 中国中医科学院中药研究所, 北京 100700
  • 2 美国乔治城大学医学中心生物化学及分子生物学系, 美国 华盛顿 20007

    • 魏梦佳,女,硕士研究生 研究方向:中药质量控制

通讯作者:

*骆璐,女,博士,助理研究员 研究方向:中药质量控制
Research on the Identification Characteristics of Synthetic and Natural Cinnabar Based on Multispectral Analyses
Mengjia Wei1, Xueying XIN1, Wenwen DUAN1, Raorao LI1, Qiaochu WANG2, Xuezhu GU1, Lu LUO1, *
Affiliations
  • 1 Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China
  • 2 Department of Biochemistry and Molecular & Cellular Biology, Georgetown University Medical Center, Washington, D.C. 20007, United States
出版时间: 2025-02-22 doi: 10.11669/cpj.2025.04.004
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摘要
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目的 研究合成朱砂和天然朱砂的晶体构型和物相组成,对比合成朱砂和天然朱砂光谱学特征,分析其显微特征及微量元素差异。方法 采用粉晶X射线衍射、拉曼光谱、傅里叶红外光谱、电子探针微区分析、电感耦合等离子体质谱等方法,探索合成朱砂和天然朱砂的鉴别方法。结果 研究表明合成朱砂和天然朱砂的晶型相同;天然朱砂中常见的杂质为石英、黄铁矿、方解石、辉锑矿等;合成朱砂中含有极少量的方解石杂质,质量较为均一;通过使用电子探针微区分析技术或粉晶X射线衍射技术结合偏光显微法,可有效对合成朱砂和天然朱砂中的杂质进行分析。结论 合成朱砂和天然朱砂的中红外光谱和拉曼光谱特征相似,其特征微量元素一致,通过等离子体电感耦合质谱法,可将铁、镁、锌3种元素作为二者鉴别的参考。

合成朱砂  /  天然朱砂  /  鉴别  /  质量控制

OBJECTIVE To investigate crystal structure and composition of synthetic and natural cinnaba,compare their spectroscopic characteristics and analyze their microscopic characteristics and trace element differences. METHODS This investigation endeavors to clarify the crystal configuration and phase composition of synthetic and natural cinnabar on the market and analyze the differences in trace elements between them. Meanwhile, we used powder X-ray diffraction, Raman spectroscopy, attenuated total reflection-Fourier transform infrared spectroscopy, electron probe micro-analysis, inductively coupled plasma mass spectrometry, with traditional microscopic identification(characteristics; optical polarized light microscopy), to explore the identification methods of synthetic and natural cinnabar. RESULTS The results suggest that, both present to share the same characteristics in the crystal forms of synthetic and natural cinnabar. Common impurities in natural cinnabar are quartz, pyrite, calcite, stibnite, etc., while the differences among different batches of samples are distinguishable. Synthetic cinnabar contains a small number of calcite impurities, and the quality is relatively uniform. By using electron probe micro-analysis technology, and powder crystal X-ray diffraction technology combined with polarized light microscopy, the impurities in synthetic cinnabar and natural cinnabar can be effectively analyzed and identified; the mid-infrared spectrum and Raman spectrum characteristics of synthetic and natural cinnabar are similar; the characteristic trace elements between synthetic and natural cinnabar are consistent. CONCLUSION Three elements including Fe, Mg and Zn can be quantified to identify these two as reference.

synthetic cinnabar  /  natural cinnabar  /  identification  /  quality control
魏梦佳, 辛雪颖, 段雯雯, 李娆娆, 王翘楚, 顾雪竹, 骆璐. 合成朱砂与天然朱砂的鉴别特征研究. 中国药学杂志, 2025 , 60 (4) : 334 -348 . DOI: 10.11669/cpj.2025.04.004
Mengjia Wei, Xueying XIN, Wenwen DUAN, Raorao LI, Qiaochu WANG, Xuezhu GU, Lu LUO. Research on the Identification Characteristics of Synthetic and Natural Cinnabar Based on Multispectral Analyses[J]. Chinese Pharmaceutical Journal, 2025 , 60 (4) : 334 -348 . DOI: 10.11669/cpj.2025.04.004
正文
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朱砂(cinnabaris),又名丹粟、朱丹、赤丹、丹砂、真朱、汞沙、光明砂、辰砂,为硫化物类矿物辰砂族辰砂,主含硫化汞(HgS)[1],具有清心镇惊,安神,明目,解毒的功效[2],主要用于治疗心悸易惊,失眠多梦,癫痫发狂,小儿惊风,视物昏花,口疮,喉痹,疮疡肿毒等症。朱砂在中医临床上应用广泛,许多中成药中都含有朱砂,如朱砂安神丸、柏子养心丸、天王补心丹等。但天然朱砂属于不可再生资源,价格昂贵,且近年来其矿产规模日趋减小,市场上出现了用合成朱砂代替天然朱砂销售和使用的现象,Ma等[3]从全国范围抽取68批次的朱砂药材,发现其中16批为合成朱砂。在我国,合成朱砂主要指灵砂和银朱,两者制备工艺不同,《天工开物》[4]记载:“凡将水银再升朱用,故名曰银朱。其法用磬口泥罐,或用上下釜。每水银一斤,入石亭脂(即硫黄制造者)二斤”。《本草纲目》[5]载:“升灵砂法:用新锅安逍遥炉上,蜜揩锅底,文火下烧,入硫黄二两熔化,投水银半斤”。现代工艺制备银朱多为水银、升华硫和氢氧化钾加热合成[6]。虽然合成朱砂制备工艺发展较为成熟,但其性味功效与天然朱砂存在较大的差异,朱砂味甘性寒,灵砂为甘温,银朱为辛温。宋代《重修政和经史证类备用本草》中[7]记载灵砂“味甘,性温,无毒”,明代《景岳全书》[8]载灵砂“味甘,性温。主上盛下虚,痰涎壅盛,头旋吐逆,霍乱反胃,心腹冷痛。升降阴阳,既济水火,久服通神明,杀精魅恶鬼,小儿惊吐”,李时珍[5]与张璐[9]均言银朱“辛,温,有毒。破积滞,劫痰涎,散结胸,疗疥癣恶疮,杀虫及虱,粉霜”。在历代古籍记载中,合成朱砂的性味功效与天然朱砂差异,在中医临床上,其代替天然朱砂使用的安全性和有效性尚不明确。目前对于朱砂的研究多集中于炮制方法、药理毒性等方面[10-11],对于合成朱砂和天然朱砂的对比性研究内容较少,且研究方向较为分散。另外,天然朱砂属于不可再生资源,价格昂贵,且近年来其矿产规模日趋减小,市场上存在合成朱砂代替天然朱砂销售和使用的现象。加之二者不易区分,给矿物药朱砂的质量控制带来了严峻的挑战。
本研究采用粉晶X射线衍射、拉曼光谱、红外光谱、电子探针、电感耦合等离子体质谱等方法,结合传统显微鉴别技术,即性状和偏光显微观察,对从市场上收集的天然朱砂和合成朱砂共计44批样品进行系统性检验测定。对比分析了合成朱砂和天然朱砂的晶体构型、显微光学、微量元素含量、光谱学特征等方面的差异,为综合评价天然朱砂与合成朱砂提供有力的数据支撑。
1 材料
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1.1 样品与试剂
朱砂样品共有44批,包括合成朱砂样品共25批和天然朱砂样品共19批,其中,来自同一产地不同批次的朱砂有1~3批次不等,见表1。元素标准液(广东华晰检测技术中心)。盐酸、硝酸、氢氟酸(优级纯,北京化工厂)。无水乙醇(分析纯,批号:20211026)。
1.2 仪器与试剂
蔡司AxioScope. A1型显微镜(德国ZEISS公司,型号:AxioScope.A1),傅里叶变换红外光谱仪(美国PerkinElmer公司,型号:ATR-Frontier),激光显微拉曼光谱仪(美国Thermo Scientific,型号:DXR 2xi),多晶X-射线衍射(德国布鲁克公司,型号:D8 Advance),电子探针X射线微区分析仪(日本岛津公司,型号:EPMA-1720H),电感耦合等离子体质谱(美国Agilent 7700型)。
无水乙醇(分析纯,批号:20211026),购自国药集团化学试剂有限公司。Ag、Al、As、Au、B、Ba、Be、Bi、Ca、Cd、Ce、Co、Cr、Cs、Cu、Dy、Er、Eu、Fe、Ga、Gd、Ge、Hf、Ho、In、Ir、K、La、Li、Lu、Mg、Mn、Mo、Na、Nb、Nd、Ni、Os、P、Pb、Pd、Pr、Pt、Rb、Re、Rh、Ru、Sb、Sc、Se、Si、Sm、Sn、Sr、Ta、Tb、Te、Th、Ti、Tl、Tm、U、V、W、Y、Yb、Zn、Zr元素标准液由广东华晰检测技术中心提供。盐酸、硝酸、氢氟酸(优级纯,北京化工厂)。
1.3 实验方法
1.3.1 偏光显微分析
工作参数:反射光源,单偏光系统;反射光源,正交偏光系统;透射光源,单偏光系统;透射光源,正交偏光系统。将44批朱砂样品分别置于玛瑙研钵中研细,200目过筛,得细粉,各取细粉少许置于试管中,滴加无水乙醇少许,用胶头滴管吸取少量混悬液在载玻片上均匀涂布,置于通风橱中,待无水乙醇挥发后,即得样品粉末标片。将块状样品经煮胶、磨片、抛光后分别制备成永久薄片,即可得到44批朱砂样品薄片标片,采用德国蔡司AxioScope. A1型显微镜对44批样品粉末及薄片显微特征进行观察和记录。
1.3.2 红外光谱分析
波数范围:4 000~400 cm-1,分辨率:4 cm-1,扫描次数3次,每个样品重复扫描3次,取平均光谱作为该样品的分析光谱。将金刚石衰减全反射(ATR)附件放置于红外光谱仪中,取样品细粉少许,置于金刚石晶体与校正压力装置之间的凹槽内,测定样品的傅立叶变换衰减全反射红外光谱法(ATR-FTIR)数据;测定前对背景进行扫描,得到的红外光谱采用自动校正方法进行基线校正;光谱扫描范围4 000~400 cm-1,仪器分辨率4 cm-1,扫描次数3次,每个样品重复扫描3次,取平均光谱作为该样品的分析光谱。
1.3.3 拉曼光谱分析
拉曼光谱仪激发光源785 nm,光谱测量范围2 700~50 cm-1,激光功率300 mV,采用激光强度30%,扫描时间100~1 000 ms,每批样品采集2次光谱并求平均,得各样品的分析光谱。
1.3.4 多晶X-射线衍射分析
工作参数:入射光源为Cu Kα辐射,Ni片滤波,工作电压40 kV,工作电流40 mA,连续式步进扫描,扫描范围:10~70°,扫描速度8 °·min-1,步长0.02 °。采用布鲁克公司EVA软件对样品的X-射线衍射原始数据进行标准化处理,并将所得衍射数据与国际标准X射线衍射数据卡片进行匹配。将采集的粉末X 射线衍射数据导入物相检索软件MDI Jade 6中进行背景扣除、平滑、拟合、寻峰等处理,得到其衍射图谱。通过MID Jade 6软件对人工和天然朱砂X射线衍射图进行物相分析,将所得衍射数据与国际粉末衍射数据中心(JCPDS)标准卡片匹配,获得物相分析结果。
1.3.5 电子探针微区(EMPA)分析
加速电压15.0 kV,束流50.0 nA,束斑直径5 μm。参照GB/T 4930-93电子探针分析标准样品通用技术条件,GB/T 15074电子探针定量分析方法通则,GB/T 15075电子探针分析仪的检测方法等国家标准进行分析。结合样品的显微特征,选取具有典型显微特征的样品片子进行电子探针分析。选取块状合成朱砂样品6批(S1、S4、S5、S7、S15、S18)及天然朱砂样品4批(N1、N3、N5、N9)经注胶成块、切片注胶、磨片清洗、黏片、磨片抛光后分别制备0.03 mm厚永久薄片。用记号笔圈定样品薄片的分析位置,在制备的显微薄片表面镀碳粉,增强其导电性,然后对每个选定位置选取5~10个典型位点测定微区成分及11个元素(Hg、S、As、Pb、Zn、Fe、Ca、Al、Mg、Na和Si)的质量分数,并根据系统矿物学指标确定矿种,并通过计算确定每个点位的主要矿物的元素组成比例,最后计算出其主要矿物相。
1.3.6 微量元素测定
采用美国Agilent 7700型电感耦合等离子体质谱对合成朱砂和天然朱砂样品进行分析。各取细粉50 mg,按照中华人民共和国国家标准GB/T14506.30—2010进行样品制备。精密称取样品,置于50 mL特氟龙消解容器中,分别加入王水6 mL、氢氟酸2 mL、双氧水1 mL,混匀,放入石墨加热板(120~200 ℃)并不断加入上述酸至样品完全消解,赶酸,冷却后定容,摇匀,用于测试。
2 结果与讨论
收起
2.1 合成和天然朱砂的外观性状鉴别
合成朱砂和天然朱砂的颜色均为鲜红色至暗红色,条痕红色,有光泽,体质量,质脆。与天然朱砂相比,合成朱砂稍显质软。合成朱砂呈块状或较大颗粒状时,可见柱状平直纵条纹;呈较小颗粒状时,部分可见条状纹理;呈细小颗粒状或粉末状时,肉眼观察无明显纹理(图1A)。合成朱砂和天然朱砂样品呈粉末状态时颜色相似,均为暗红色,有光泽,外观性状无显著区别(图1B)。
2.2 偏光显微观察分析
2.2.1 合成和天然朱砂的粉末显微特征
在反射正交偏光下,合成朱砂与天然朱砂的晶体颜色均为樱红色至红色,不透明或半透明。合成朱砂晶体常黏结成团块状,少见白色方解石杂质,可见白色透明圆球状杂质;天然朱砂中多见白色方解石杂质,且方解石常散在或嵌合于成团块状朱砂晶体内,少见白色透明圆球状杂质。
在反射正交偏光下,可观察到合成朱砂的晶体呈樱红色至红色,半透明或不透明,形态多为团块状;少见白色方解石杂质,多散在;可见白色透明圆球状杂质,多独立或凝集成葡萄状。合成朱砂样品粉末的偏光显微特征图,见图2。
在反射正交偏光下,天然朱砂的晶体呈樱红色至红色,半透明或不透明,多散在或呈团块状;可见白色方解石杂质,多嵌合于成团块状朱砂晶体内;少见白色透明圆球状杂质。在样品N7、N8、N9、N10、N13、N16、N17、N18和N19的粉末标片中,未观察到白色透明圆球状杂质。天然朱砂样品粉末的偏光显微特征图,见图3。
2.2.2 合成和天然朱砂的薄片显微特征
在反射正交偏光下,合成与天然朱砂薄片呈樱红色或橘红色,在透射正交偏光下呈红色至暗红色。合成朱砂薄片在反射正交偏光下可见亮白色杂质,未观察到明显伴生矿物;天然朱砂薄片在透射光下多见石英、方解石等伴生矿物。
在反射正交偏光下,合成朱砂薄片呈樱红色或橘红色,可见亮白色杂质;多数薄片标片有纵纹或细直条纹裂隙。在透射正交偏光下,合成朱砂薄片呈红色至暗红色,可见纵纹或细直条纹裂隙。合成朱砂样品薄片的反射、透射正交偏光偏光显微特征图,见图4。
在反射正交偏光下,天然朱砂薄片呈樱红色或橘红色;多数薄片标片有伴生矿物。在透射正交偏光下,天然朱砂薄片呈红色至暗红色,可见多种伴生矿物。天然朱砂样品薄片的反射、透射正交偏光偏光显微特征图,见图5。
2.3 合成和天然朱砂的光谱特征分析
2.3.1 合成和天然朱砂的红外光谱特征分析
红外光谱在矿物药的研究中有着广泛的应用,属于分子吸收光谱,具有高度的专属性[9]。中红外光谱测试结果显示[1012-13],合成朱砂和天然朱砂在2 001、1 000 cm-1附近有共有峰,2 001 cm-1处为二氧化碳吸收峰,1 000 cm-1处为二氧化硅吸收峰。合成与天然朱砂样品在2 600~2 000 cm-1处有二氧化碳特征吸收带,在1 500~1 416和667 cm-1附近有碳酸盐特征吸收,在484~407 cm-1处有石英特征吸收带(图6A)。天然朱砂部分样品在1 424、877、728和1 416、875 cm-1处有方解石吸收峰,在1 442~1 469 cm-1处有白云石特征吸收(图6B)。在中红外波段4 000~400 cm-1下,合成朱砂与天然朱砂主矿物相硫化汞的光谱特征不明显,其他物质如二氧化硅、石英和方解石等在该波段下的吸收较强。
2.3.2 合成和天然朱砂的拉曼光谱特征分析
25批合成朱砂拉曼光谱图(图6C),在86 cm-1拉曼位移处的平均强度为496,在104 cm-1拉曼位移处的平均强度为658,在143 cm-1拉曼位移处的平均强度为204,在254 cm-1拉曼位移处的平均强度为7 098,在285 cm-1拉曼位移处的平均强度为935,在343 cm-1拉曼位移处的平均强度为1 972。样品S4在343、285、254、143、104、86 cm-1拉曼位移处的强度均为最低,样品S25在上述拉曼位移处的强度均为最高,极差值分别为2 981、1 470、9 878、322、1 073、857。25批合成朱砂样品在254 cm-1处的极差值最大,在143 cm-1处的极差值最小。
19批天然朱砂拉曼光谱图(图6D),在86 cm-1拉曼位移处的平均强度为917,在104 cm-1拉曼位移处的平均强度为1 208,在143 cm-1拉曼位移处的平均强度为411,在254 cm-1拉曼位移处的平均强度为12 047,在285 cm-1拉曼位移处的平均强度为1 689,在343 cm-1拉曼位移处的平均强度为3 478。样品N12在343、285、254、143、104、86 cm-1拉曼位移处的强度均为最低。样品N10在343、254、104 cm-1拉曼位移处的强度均为最高,极差值分别为3 593、11 718、1 266;样品N19在143、86 cm-1拉曼位移处的强度均为最高,极差值分别为579、869;样品N9在285 cm-1拉曼位移处的强度均为最高,极差值分别为1 586。19批天然朱砂样品在254 cm-1处的极差值最大,在143 cm-1处的极差值最小。
采用了两种方法检验两组之间的差异。第一种方法计算每个拉曼位移的平均强度,并在样品平均值之间进行Wilcoxon符号秩检验。第二种方法将每个拉曼位移投影到第一主成分上,并在来自每个组的第一主成分得分之间执行双样本Wilcoxon秩和检验。对于第一种方法,计算每个组的每个拉曼位移的样本之间的平均强度(图7)。
由图7A、C可见大多数样本彼此高度相关。每个拉曼位移的平均强度差异的Shapiro-Wilk正态性检验产生的P<0.000 1,导致拒绝配对差异遵循正态分布的零假设。因此,本研究选择Wilcoxon符号秩检验。还发现所得P<0.000 1,这提供了强有力的证据,表明N组的强度测量值显著大于S组。下面的箱形图显示了每个拉曼位移的平均强度,说明组N通常具有较大的测量值。
首先将每个拉曼位移投影到第一主成分上。如图7B、D所示,第一主成分解释了数据中69.8%的变异。然后,对每组的主成分评分进行了Shapiro-Wilk正态性检验,每种情况下的P值均小于0.01。因此,拒绝了数据来自正态分布的零假设。由于不符合双样本t检验的假设,进行了双侧Wilcoxon秩和检验,检验两组之间的差异。所得P<0.000 1,为每组强度测量值之间的差异提供了有力证据。进一步分析发现:合成朱砂和天然朱砂的拉曼光谱特征峰主要为343、285、254、143、104、86 cm-1。天然朱砂在343、285、254、143、104、86 cm-1拉曼位移处的平均强度均高于合成朱砂。
2.4 合成和天然朱砂的物相组成分析
2.4.1 粉晶X射线衍射物相检索结果及分析
将采集的粉末X 射线衍射数据导入物相检索软件MDI Jade 6中进行背景扣除、平滑、拟合、寻峰等处理,得到其衍射图谱(图8)。
通过MID Jade 6软件对人工和天然朱砂X射线衍射图进行物相分析,将所得衍射数据与国际粉末衍射数据中心JCPDS标准卡片匹配,获得物相分析结果。通过对各样品的物相分析、检索匹配可知,人工和天然朱砂样品的主要物相均为α-型硫化汞(HgS)。合成朱砂和天然朱砂的粉末X射线衍射图谱的物相检索结果显示:25批合成朱砂与19批天然朱砂的晶体均为硫化汞,属于六方晶系(hexagonal),均为α-型硫化汞。
在合成朱砂样品中,仅S14和S13的空间群为P3221(154),PDF#标准卡片为80-2192(晶格常数:a=4.145,b=4.145,c=9.496,α=90.0,β=90.0,γ=120.0),其他23批样品的空间群均为P3121(152),PDF#标准卡片为99-0031(晶格常数:a=4.149,b=4.149,c=9.495,α=90.0,β=90.0,γ=120.0);在天然朱砂样品中,所有样品的空间群均为P3121(152),除N14的PDF#标准卡片为89-0438(晶格常数:a=4.131 7,b=4.131 7,c=9.445 1,α=90.0,β=90.0,γ=120.0)外,其他13批样品的PDF#标准卡片均为99-0031(晶格常数:a=4.149,b=4.149,c=9.495,α=90.0,β=90.0,γ=120.0)。
合成朱砂和天然朱砂的物相一致,晶体构型相同。与天然朱砂相比,25批合成朱砂的晶粒尺寸数值较为均一,平均值为1 457 Å,最大值为S2样品的2 470 Å,最小值为S12样品的679 Å,极差值为1 791 Å;而19批天然朱砂晶粒尺寸的平均值为1 187 Å,最大值为N1样品的3 751 Å,最小值为N15样品的583 Å,极差值为3 168 Å。合成朱砂和天然朱砂在微观应力值方面的数据特征与晶粒尺寸相似,合成朱砂微观应力均值为0.119%,最大值为S2的0.155%,最小值为S12的0.068%,极差值为0.087%;天然朱砂微观应力均值为0.077%,最大值为N1的0.131%,最小值为N15的0.014%,极差值为0.117%。见表2。
2.4.2 EMPA分析
选取合成朱砂和天然朱砂典型样品进行EMPA定性和定量测定,并对检测结果进行分析。对上述样品的主要矿物相硫化汞进行定量分析,结果表明,合成朱砂与天然朱砂硫化汞相的主量元素均为Hg和S,且汞硫元素比接近1∶1。
合成朱砂的矿物相为硫化汞,较为纯净。在EMPA定量检测中,6批样品S1、S4、S5、S7、S15、S18矿物相硫化汞的Hg和S元素含量比均值为49∶50。在9种微量元素中,样品均未检测到Si元素,S4、S5、S7、S15样品中均未检测到Na元素。As、Fe、Na、Al这4种元素的平均含量较低(分别为0.003%、0.007%、0.003%、0.007%),Zn、Mg、Pb、Ca这4种元素的平均含量较高(分别为0.044%、0.062%、0.064%、0.017%)(图9)。
天然朱砂的主要矿物相为硫化汞,此外,还含有其他伴生矿物。在EMPA定性分析中,4批样品N1、N3、N5、N9含有石英、黄铁矿、方解石、辉锑矿、白云石等伴生矿物。通过EMPA分析法对4批天然朱砂样品的主要矿物相硫化汞微区进行定量检测,结果表明,Hg元素和S元素含量比均值为49∶50。在9种微量元素中,样品N5、N9未检测到Si元素,样品N3、N5未检测到Na元素,样品N3未检测到Al元素。As、Si、Fe、Na、Ca这5种元素的平均含量较低(分别为0.003%、0.018%、0.005%、0.001%、0.013%),Zn、Al、Mg、Pb这4种元素的平均含量较高(分别为0.046%、0.031%、0.070%、0.063%)(图10)。
2.5 合成和天然朱砂的微量元素分析
合成朱砂和天然朱砂的等离子体电感耦合质谱分析结果见表3。在天然朱砂中,Sb元素的平均含量最高,Be元素的平均含量最低。在合成朱砂中,Ca元素的平均含量最高,Be元素的平均含量最低。合成朱砂B、Cu、Pd、Tl、Zr元素的平均含量高于天然朱砂,其他微量元素平均含量均低于天然朱砂。其中,天然朱砂有10种微量元素的平均含量是合成朱砂的一百倍及以上,即元素As、Cd、Fe、Mg、Mn、Pb、Sb、Se、Sn、Zn,分别为合成朱砂的105.93、451.23、382.22、331.68、350.26、169.99、1156.58、498.66、393.01、323.09倍;天然朱砂有6种微量元素的平均含量是合成朱砂的十倍及以上,即元素Rh、Ca、Ba、La、Cr、Sr,分别为合成朱砂的91.09、40.71、34.76、32.42、19.07、11.63倍;天然朱砂其他47种微量元素的平均含量是合成朱砂的1.06~8.05倍(图11A)。对各种元素进行对比分析发现,合成和天然朱砂的As、Cd、Fe、Mg、Mn、Pb、Sb、Se、Sn、Zn的元素含量存在较大差异,可将上述10种元素作为区分合成朱砂和天然朱砂的参考。
运用SPSS Statistics 17.0软件对25批合成朱砂和19批天然朱砂样品的68种微量元素含量数据进行主成分分析,以确定其特征元素。68种微量元素即68个成分,为方便运算,均使用阿拉伯数字1~68代指(即1Ag、2Al、3As、4Au、5B、6Ba、7Be、8Bi、9Ca、10Cd、11Ce、12Co、13Cr、14Cs、15Cu、16Dy、17Er、18Eu、19Fe、20Ga、21Gd、22Ge、23Hf、24Ho、25In、26Ir、27K、28La、29Li、30Lu、31Mg、32Mn、33Mo、34Na、35Nb、36Nd、37Ni、38Os、39P、40Pb、41Pd、42Pr、43Pt、44Rb、45Re、46Rh、47Ru、48Sb、49Sc、50Se、51Si、52Sm、53Sn、54Sr、55Ta、56Tb、57Te、58Th、59Ti、60Tl、61Tm、62U、63V、64W、65Y、66Yb、67Zn、68Zr)。由表3可知,前15个成分的累积方差贡献率为90.357%>90%,即1个15成分因子的模型解释了90.357%的实验数据。由于因子过多,可剔除主成分第一列合计特征值小于1的因子,第1至14个因子在此列的特征值均大于1,因此,可剔除因子15,保留因子1~14。由图11B碎石图可观察到,在成分14处特征值出现明显的转折,且已包含大量信息,因此,结合表2相关信息,选择14因子模型。由表4旋转成分矩阵数据可知,第1主因子与元素Cd、Fe、Pt、Rh、Sn、Tm高度相关,第2主因子与元素Ce、In、La、Nd、Y高度相关,第3主因子与元素Co、Cs、Ni高度相关,第4主因子与元素Al高度相关,因为前4个主因子的累积方差贡献率已超过50%,所以可以认为Cd、Fe、Pt、Rh、Sn、Tm、Ce、In、La、Nd、Y、Co、Cs、Ni、Al是合成和天然朱砂的特征微量元素(图11B)。
采用了两种方法检验两组之间的差异(图11C~D)。第一种方法涉及计算每个元素的样本平均测量值,并在样本平均值之间进行配对t检验和Wilcoxon符号秩检验。第二种方法涉及基于排列的方法,以确定从单个测试获得的P值是否足够小,以至于随机发生。第一种方法,计算每组样本每个元素的平均含量。下面的相关图证明,表明大多数样本彼此高度相关。每个元素平均含量差异的Shapiro-Wilk正态性检验得出的P=0.201,导致配对差异遵循正态分布的零假设被拒绝。因此,符合配对t检验的假设。发现所得P<0.000 1,表明N组的强度测量值显著大于S组。箱形图显示了每个元素的平均含量,说明组N通常具有较大的测量值。Wilcoxon符号秩检验也导致P<0.000 1(图11E)。
同时进行了70个单独的单侧t检验,以比较每个元素的样本测量值。这些检验的平均P值为0.246,如P值直方图所示(图11F)。为了评估该平均P值的统计显著性,本研究使用基于排列的方法。对于每个元素,本研究随机排列40个测量值,将前25个分配给S组,剩余的19个分配给N组。然后本研究计算70次测试的平均P值。最后,本研究将P值确定为模拟平均P值小于0.246的次数(1 000次重复)的比例。所得P值为0,表明N组的测量值显著大于S组的强有力证据。为了确定哪些元素在N组中的测量值显著大于S组,本研究进行了70次单独的t检验,并使用Bonferroni校正调整了P值,以考虑多重比较。通过70次检验,调整后的显著性水平约为0.05/70×0.000 71。只有元素Au的P值低于该调整阈值,表明N组的测量值显著大于S组。图11G显示了具有10个最小P值的每组元素的测量值。
3 讨论
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采用偏光显微特征进行对比分析发现,在反射正交偏光下,合成朱砂中方解石少见且多散在,可见白色透明圆球状杂质;天然朱砂中方解石常嵌合于成团块状朱砂晶体内,少见白色透明圆球状杂质。薄片偏光显微特征表明,合成朱砂中常见纵纹或细直条纹裂隙。在反射正交偏光下,合成朱砂和天然朱砂薄片呈樱红色或橘红色,合成朱砂薄片中可见亮白色杂质;在透射正交偏光下,合成朱砂和天然朱砂薄片呈红色至暗红色,天然朱砂中多见石英、方解石等伴生矿物。可见偏光显微特征,特别是薄片的显微特征,可初步鉴别合成朱砂和天然朱砂。
采用粉晶X射线衍射技术对比分析,发现合成朱砂和天然朱砂的晶体构型相同,均属于α-型硫化汞,不同批次合成朱砂的晶粒尺寸值和微观应力值更加均一,而不同批次的天然朱砂的晶粒尺寸值和微观应力值的差异较大,可进一步鉴别合成朱砂和天然朱砂。
采用电子探针微区定性和定量技术对比分析,发现合成朱砂和天然朱砂的主要矿物相均为硫化汞,其中,合成朱砂较为纯净,而天然朱砂中含有石英、黄铁矿、方解石、辉锑矿、白云石等伴生矿物。在硫化汞相中二者的主量元素均为Hg和S,合成朱砂样品均未检测到Si元素,其他微量元素的含量差异不大。可见,EMPA分析不适用于合成朱砂和高纯度天然朱砂的鉴别。
采用傅里叶变换红外光谱法和激光拉曼光谱法对合成朱砂和天然朱砂的光谱特对比分析,发现合成和天然朱砂主矿物相硫化汞在中红外区的光谱特征不明显,其他物质如二氧化硅、石英和方解石等在该波段下的吸收较强。合成朱砂和天然朱砂的拉曼光谱特征峰主要为343、285、254、143、104、86 cm-1,且天然朱砂在上述拉曼位移处的平均强度值和极差值均高于合成朱砂,合成朱砂和天然朱砂的中红外和拉曼光谱相似。可见,通过光谱特征对合成和天然朱砂进行鉴别较为困难。
采用等离子体电感耦合质谱法分析,发现合成朱砂和天然朱砂的特征微量元素是Cd、Fe、Pt、Rh、Sn、Tm、Ce、In、La、Nd、Y、Co、Cs、Ni、Al。合成朱砂B、Cu、Pd、Tl、Zr元素的平均含量高于天然朱砂,其他微量元素平均含量均低于天然朱砂,二者的As、Cd、Fe、Mg、Mn、Pb、Sb、Se、Sn、Zn的元素含量存在较大差异。结合Ma等[3]的研究发现,可将Fe、Mg、Zn 3种元素作为合成和天然朱砂鉴别的参考。
4 结论
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本研究主要讨论合成和天然朱砂的鉴别特征。采用X射线衍射等方法,结合传统显微鉴别技术,为合成朱砂和天然朱砂的鉴别和矿物药朱砂的质量控制提供参考。本研究提供了合成朱砂和天然朱砂新检验流程:第一步:通过外观性状作为初步鉴别合成朱砂和天然朱砂的依据。第二步:偏光显微结合XRD技术确定朱砂样品的晶型后,可对合成和天然朱砂进行进一步且较为准确的鉴别。第三步:通过等离子体电感耦合质谱法进行铁、镁、锌3种元素的测量来鉴别合成和天然朱砂。通过EMPA技术分析矿物相组成,可对合成和天然朱砂进行区分。通过以上检测步骤的综合运用,可对合成朱砂和天然朱砂形成更为准确的检测和区分。本研究同时还发现以下几种检测方式不适于鉴别合成和天然朱砂。①EMPA可能不适用于鉴别合成朱砂和高纯度的天然朱砂;②傅里叶变换红外光谱法和激光拉曼光谱法无法准确对合成和天然朱砂进行鉴别;当前对朱砂的研究多集中于炮制方法、药理毒性等,而缺少合成朱砂和天然朱砂鉴别的方法,本研究采用多种鉴别方法,创新性地提出了合成朱砂和天然朱砂的新检验流程,弥补了缺少对朱砂质量标准,从而进一步探索合成朱砂和天然朱砂在临床使用中的有效性和安全性研究奠定了基础。
基金
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  • 国家自然科学基金青年科学基金项目资助(82204610)
  • 中国中医科学院科技创新工程项目资助(C12021A04013)
文献
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参考文献 引证文献
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2025年第60卷第4期
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doi: 10.11669/cpj.2025.04.004
  • 接收时间：2024-07-24
  • 首发时间：2025-11-07
  • 出版时间：2025-02-22
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  • 收稿日期：2024-07-24
基金
国家自然科学基金青年科学基金项目资助(82204610)
中国中医科学院科技创新工程项目资助(C12021A04013)
作者信息
    1 中国中医科学院中药研究所, 北京 100700
    2 美国乔治城大学医学中心生物化学及分子生物学系, 美国 华盛顿 20007

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*骆璐,女,博士,助理研究员 研究方向:中药质量控制
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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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