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Article(id=1195664140745356284, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195664138694341616, articleNumber=1001-2494(2024)02-0179-07, orderNo=null, doi=10.11669/cpj.2024.02.010, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1685462400000, receivedDateStr=2023-05-31, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1762998145518, onlineDateStr=2025-11-13, pubDate=1705852800000, pubDateStr=2024-01-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1762998145518, onlineIssueDateStr=2025-11-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1762998145518, creator=13701087609, updateTime=1762998145518, updator=13701087609, issue=Issue{id=1195664138694341616, tenantId=1146029695717560320, journalId=1190317699101192196, year='2024', volume='59', issue='2', pageStart='101', pageEnd='190', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1762998145030, creator=13701087609, updateTime=1762998511460, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1195665675697045692, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195664138694341616, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1195665675701239997, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195664138694341616, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=179, endPage=185, ext={EN=ArticleExt(id=1195664140929905662, articleId=1195664140745356284, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Determination of Trace Elements in Cistanches Herba from Different Habitats by ICP-MS, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To establish a method for the determination of 37 kinds of inorganic elements by microwave digestion and inductively coupled plasma mass spectrometer (ICP-MS), and to detect and analyze 37 kinds of inorganic elements in cistanches herba from different habitats, and to preliminatively explore the pollution distribution of various inorganic elements in cistanches herba from different habitats. METHODS Using nitric acid and hydrogen peroxide as digestion reagent, microwave digestion was used to pretreat the samples. The contents of 37 inorganic elements in cistanches herba were determined simultaneously by internal standard correction and external standard quantitative ICP-MS method. RESULTS In the curve range of 0.50-100 μg·L-1(Hg: 0.20-20 μg·L-1) showed a good linear relationship with the peak area (r≥0.997 4). The detection limits were 0.000 27-0.045 μg·L-1. The average recoveries were 76.5% to 110.0% at high, medium and low levels. RSD of precision and repeatability were lower than 4.8%. The detection rates of 5 harmful heavy metal elements (copper, lead, arsenic, mercury, cadmium) that need to be controlled by Chinese Pharmacopoeia (2015 edition) in 40 batches of cistanches herba were 27.5%, 7.5%, 82.5%, 0 and 100%, respectively. The detection rate of barium, manganese, rubidium and strontium in 40 batches of samples is 100%, and the content is much higher than other elements,there are obvious regional differences. CONCLUSION This method has high sensitivity, good reproducibility, reduced the inspection time and cost, and can simultaneously detect various inorganic elements in cistanches herba, providing data support for optimal cultivation, quality assurance and drug safety of cistanches herba.

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目的 建立37种元素的微波消解-电感耦合等离子体质谱(ICP-MS)测定方法,并对不同产地的肉苁蓉中37种无机元素进行检测分析,初步探索研究不同产地肉苁蓉中多种无机元素的污染分布情况。方法 以硝酸-过氧化氢为消解试剂,采用微波消解法对样品进行前处理,通过采用在线内标校正,外标法定量ICP-MS 法同时测定肉苁蓉中37种无机元素的含量。结果 在曲线范围0.50~100 μg·L-1(Hg:0.20~20 μg·L-1)内与峰面积呈良好的线性关系(r≥0.997 4),检出限为0.000 27~0.045 μg·L-1,加标回收率在高、中、低3 个添加水平下,元素的平均回收率介于76.5%~110.0%,仪器精密度和重复性的相对标准偏差(RSD)值均<4.8%;40批肉苁蓉中5种《中国药典》2020年版明确需要控制的有害重金属元素(铜、铅、砷、汞、镉)的检出率分别为27.5%、7.5%、82.5%、0和100%;钡元素、锰元素、铷元素和锶元素在 40 批样品检出率均为100%,且含量远远高于其他元素,具有明显的地域性差异。结论 该方法灵敏度高、重现性好、缩短了检验时间、降低了检验成本,可同时检测肉苁蓉中多种无机元素,为肉苁蓉的优化培育和保证药材品质以及用药安全提供数据支撑。

, correspAuthors=孙莺, authorNote=null, correspAuthorsNote=
*孙莺,女,博士,主任药师 研究方向:药品质量控制 Tel:(0931)7822939
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徐勤科,男,硕士,高级工程师 研究方向:药品质量控制及标准研究

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徐勤科,男,硕士,高级工程师 研究方向:药品质量控制及标准研究

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徐勤科,男,硕士,高级工程师 研究方向:药品质量控制及标准研究

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Food Sci Technol(食品科技), 2019, 46(12):76-81., articleTitle=Application of Cistanche in health food in China, refAbstract=null), Reference(id=1197097900124713445, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, doi=null, pmid=null, pmcid=null, year=2002, volume=41, issue=3, pageStart=278, pageEnd=281, url=null, language=null, rfNumber=[8], rfOrder=7, authorNames=WU ZH Y, LIU L Y, AI L F, journalName=Hydrometallurgy(湿法冶金), refType=null, unstructuredReference=WU ZH Y, LIU L Y, AI L F. Simultaneous determination of 16 rare earth elements in traditional Chinese medicine by microwave digestion and ICP-MS[J]. Hydrometallurgy(湿法冶金), 2002, 41(3):278-281., articleTitle=Simultaneous determination of 16 rare earth elements in traditional Chinese medicine by microwave digestion and ICP-MS, refAbstract=null), Reference(id=1197097900204405222, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, doi=null, pmid=null, pmcid=null, year=2022, volume=43, issue=5, pageStart=318, pageEnd=322, url=null, language=null, rfNumber=[9], rfOrder=8, authorNames=ZHANG G X, HU Q X, LI G, journalName=Food Ind(食品工业), refType=null, unstructuredReference=ZHANG G X, HU Q X, LI G. Determination of 27 inorganic elements in Quinoa from different origin by ICP-MS[J]. Food Ind(食品工业), 2022, 43(5):318-322., articleTitle=Determination of 27 inorganic elements in Quinoa from different origin by ICP-MS, refAbstract=null), Reference(id=1197097900376371687, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, doi=null, pmid=null, pmcid=null, year=null, volume=51, issue=3, pageStart=256, pageEnd=264, url=null, language=null, rfNumber=[10], rfOrder=9, authorNames=XU Q K, WEI P, GUO Z H, journalName=Daily Use Chem Ind(日用化学工业), refType=null, unstructuredReference=XU Q K, WEI P, GUO Z H, et al. Determination of 37 trace elements in lipstick by microwave digestion and inductively coupled plasma mass spectrometry[J]. Daily Use Chem Ind(日用化学工业),21, 51(3):256-264., articleTitle=Determination of 37 trace elements in lipstick by microwave digestion and inductively coupled plasma mass spectrometry, refAbstract=null), Reference(id=1197097900447674856, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, doi=null, pmid=null, pmcid=null, year=2021, volume=11, issue=6, pageStart=107, pageEnd=113, url=null, language=null, rfNumber=[11], rfOrder=10, authorNames=JIANG J H, XU X Z, WANG L L, journalName=Chin J Inor Anal Chem(中国无机分析化学), refType=null, unstructuredReference=JIANG J H, XU X Z, WANG L L, et al. Determination of 18 trace elements in sulfur by microwave digestion and inductively coupled plasma mass spectrometry (ICP-MS)[J]. Chin J Inor Anal Chem(中国无机分析化学), 2021, 11(6):107-113., articleTitle=Determination of 18 trace elements in sulfur by microwave digestion and inductively coupled plasma mass spectrometry (ICP-MS), refAbstract=null), Reference(id=1197097900510589417, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, doi=null, pmid=null, pmcid=null, year=2019, volume=41, issue=11, pageStart=3618, pageEnd=3624, url=null, language=null, rfNumber=[12], rfOrder=11, authorNames=LIU Q R, DU Z W, LI J Z, journalName=Spectrosc Spectral Anal(光谱学与光谱分析), refType=null, unstructuredReference=LIU Q R, DU Z W, LI J Z, et al. Analysis and evaluation of inorganic elements in Salvia miltiorrhiza and rhizosphere soil from different habitats[J]. Spectrosc Spectral Anal(光谱学与光谱分析), 2019, 41(11):3618-3624., articleTitle=Analysis and evaluation of inorganic elements in Salvia miltiorrhiza and rhizosphere soil from different habitats, refAbstract=null), Reference(id=1197097900590281194, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, doi=null, pmid=null, pmcid=null, year=2023, volume=58, issue=5, pageStart=391, pageEnd=395, url=null, language=null, rfNumber=[13], rfOrder=12, authorNames=LI Y L, LIN Z J, ZHANG B, journalName=Chin Pharm J(中国药学杂志), refType=null, unstructuredReference=LI Y L, LIN Z J, ZHANG B, et al. Study on total arsenic and its morphology and valence state in Cordyceps[J]. Chin Pharm J(中国药学杂志), 2023, 58(5):391-395., articleTitle=Study on total arsenic and its morphology and valence state in Cordyceps, refAbstract=null)], funds=[Fund(id=1197097899482984925, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, awardId=2020GSMPA-KL08, language=CN, fundingSource=2020年中药材及饮片质量控制重点实验室项目资助(2020GSMPA-KL08), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1197097896857350572, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, xref=null, ext=[AuthorCompanyExt(id=1197097896865739181, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, companyId=1197097896857350572, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Gansu Pharmaceutical Inspection Institute, Lanzhou 730000, China), AuthorCompanyExt(id=1197097896874127790, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, companyId=1197097896857350572, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=甘肃省药品检验研究院, 兰州 730000)])], figs=[ArticleFig(id=1197097898832867797, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=EN, label=Tab.1, caption=

Sample pretrentment using microwave digestion procedure

, figureFileSmall=null, figureFileBig=null, tableContent=
t/min Power/W T/℃
0-10 1 200 180
10-15 1 200 210
15-25 1 200 210
25-35 1 200 80
), ArticleFig(id=1197097898891588054, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=CN, label=表1, caption=

样品前处理微波消解程序

, figureFileSmall=null, figureFileBig=null, tableContent=
t/min Power/W T/℃
0-10 1 200 180
10-15 1 200 210
15-25 1 200 210
25-35 1 200 80
), ArticleFig(id=1197097898946114007, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=EN, label=Tab.2, caption=

Linear range, correlation coefficient, detection limit and quantitative limit of 37 trace elements standard curves

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial number Element Linear equation Linear range/μg·L-1 Correlation coefficientr LOD/mg·kg-1 LOQ/mg·kg-1
1 Ag107 C=0.057 471 4I+0.066 906 7 0.50-100 0.999 9 0.000 5 0.001
2 As75 C=1.347 774I-0.246 076 9 0.50-100 0.999 8 0.004 0.01
3 Ba137 C=0.068 003 0I-0.368 938 7 0.50-100 0.999 9 0.001 0.004
4 Be9 C=440.571 4I-0.057 632 9 0.50-100 0.999 9 0.000 07 0.000 2
5 Bi209 C=0.023 304 5I+0.561 363 5 0.50-100 0.999 3 0.001 0.005
6 Cd111 C=0.126 948 7I+0.112 984 4 0.50-100 0.999 9 0.000 07 0.000 2
7 Ce140 C=0.031 745 9I+0.225 377 0 0.50-100 0.999 9 0.000 2 0.000 6
8 Co59 C=0.171 992 0I+0.280 299 6 0.50-100 0.999 9 0.000 7 0.002
9 Cr52 C=0.289 017 3I-0.149 617 2 0.50-100 0.999 8 0.002 0.005
10 Cs133 C=0.045 328 4I+0.154 665 2 0.50-100 0.999 9 0.000 06 0.000 2
11 Cu63 C=0.231 053 8I-6.636 678 0.50-100 0.999 8 0.009 0.03
12 Dy163 C=0.058 106 2I+0.075 143 9 0.50-100 0.999 9 0.000 05 0.000 2
13 Er166 C=0.051 954 8I+0.024 537 5 0.50-100 0.999 9 0.000 3 0.001
14 Eu153 C=0.048 790 7I+0.295 233 7 0.50-100 0.999 9 0.000 08 0.000 3
15 Gd157 C=0.085 909 0I+0.261 322 6 0.50-100 0.999 9 0.000 2 0.000 7
16 Hg202 C=0.153 872 7I+0.380 189 2 0.20-20 0.997 4 0.000 7 0.002
17 Ho165 C=0.016 883 7I+0.391 279 8 0.50-100 0.999 7 0.000 2 0.000 6
18 In115 C=0.045 020 4I+0.137 330 8 0.50-100 0.999 9 0.000 05 0.000 2
19 La139 C=0.036 394 4I+0.196 851 0 0.50-100 0.999 9 0.000 4 0.001
20 Li7 C=1 026.178I+0.256 840 8 0.50-100 0.999 8 0.000 05 0.000 2
21 Lu175 C=0.023 153 9I+0.032 032 9 0.50-100 0.999 9 0.000 2 0.000 6
22 Mn55 C=0.469 072 4I+0.125 211 9 0.50-100 0.999 8 0.001 0.005
23 Nd146 C=0.074 743 6I+0.319 813 5 0.50-100 0.999 9 0.000 06 0.000 2
24 Ni60 C=0.284 332 1I-0.233 760 7 0.50-100 0.999 8 0.002 0.006
25 Pb208 C=0.039 093 5I-0.541 734 8 0.50-100 0.999 9 0.001 0.004
26 Pr141 C=0.029 440 0I+0.413 322 3 0.50-100 0.999 8 0.000 06 0.000 2
27 Rb85 C=0.594 836 4I+0.364 683 6 0.50-100 0.999 9 0.000 3 0.000 8
28 Sc45 C=1.183 274I+0.498 099 5 0.50-100 0.999 8 0.000 5 0.002
29 Sm147 C=0.093 714 1I+0.373 438 3 0.50-100 0.999 9 0.000 1 0.000 4
30 Sr88 C=0.250 044 5I+0.283 439 7 0.50-100 0.999 8 0.001 0.004
31 Tb159 C=0.017 194 5I+0.329 0511 0.50-100 0.999 8 0.000 2 0.000 7
32 Th232 C=0.027 729 3I+0.189 597 5 0.50-100 0.999 9 0.000 4 0.001
33 Tl205 C=0.027 957 4I-0.148 459 4 0.50-100 0.999 9 0.000 6 0.000 2
34 Tm169 C=0.020 832 4I+0.655 435 6 0.50-100 0.999 3 0.000 07 0.000 2
35 V51 C=0.382 192 9I+0.376 613 7 0.50-100 0.999 9 0.000 3 0.000 8
36 Y89 C=0.114 733 4I+0.318 146 4 0.50-100 0.999 9 0.000 1 0.000 4
37 Yb172 C=0.050 401 8I+0.049 465 6 0.50-100 0.999 9 0.000 3 0.000 9
), ArticleFig(id=1197097899034194392, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=CN, label=表2, caption=

37种微量元素标准曲线线性范围、相关系数、检出限和定量限

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial number Element Linear equation Linear range/μg·L-1 Correlation coefficientr LOD/mg·kg-1 LOQ/mg·kg-1
1 Ag107 C=0.057 471 4I+0.066 906 7 0.50-100 0.999 9 0.000 5 0.001
2 As75 C=1.347 774I-0.246 076 9 0.50-100 0.999 8 0.004 0.01
3 Ba137 C=0.068 003 0I-0.368 938 7 0.50-100 0.999 9 0.001 0.004
4 Be9 C=440.571 4I-0.057 632 9 0.50-100 0.999 9 0.000 07 0.000 2
5 Bi209 C=0.023 304 5I+0.561 363 5 0.50-100 0.999 3 0.001 0.005
6 Cd111 C=0.126 948 7I+0.112 984 4 0.50-100 0.999 9 0.000 07 0.000 2
7 Ce140 C=0.031 745 9I+0.225 377 0 0.50-100 0.999 9 0.000 2 0.000 6
8 Co59 C=0.171 992 0I+0.280 299 6 0.50-100 0.999 9 0.000 7 0.002
9 Cr52 C=0.289 017 3I-0.149 617 2 0.50-100 0.999 8 0.002 0.005
10 Cs133 C=0.045 328 4I+0.154 665 2 0.50-100 0.999 9 0.000 06 0.000 2
11 Cu63 C=0.231 053 8I-6.636 678 0.50-100 0.999 8 0.009 0.03
12 Dy163 C=0.058 106 2I+0.075 143 9 0.50-100 0.999 9 0.000 05 0.000 2
13 Er166 C=0.051 954 8I+0.024 537 5 0.50-100 0.999 9 0.000 3 0.001
14 Eu153 C=0.048 790 7I+0.295 233 7 0.50-100 0.999 9 0.000 08 0.000 3
15 Gd157 C=0.085 909 0I+0.261 322 6 0.50-100 0.999 9 0.000 2 0.000 7
16 Hg202 C=0.153 872 7I+0.380 189 2 0.20-20 0.997 4 0.000 7 0.002
17 Ho165 C=0.016 883 7I+0.391 279 8 0.50-100 0.999 7 0.000 2 0.000 6
18 In115 C=0.045 020 4I+0.137 330 8 0.50-100 0.999 9 0.000 05 0.000 2
19 La139 C=0.036 394 4I+0.196 851 0 0.50-100 0.999 9 0.000 4 0.001
20 Li7 C=1 026.178I+0.256 840 8 0.50-100 0.999 8 0.000 05 0.000 2
21 Lu175 C=0.023 153 9I+0.032 032 9 0.50-100 0.999 9 0.000 2 0.000 6
22 Mn55 C=0.469 072 4I+0.125 211 9 0.50-100 0.999 8 0.001 0.005
23 Nd146 C=0.074 743 6I+0.319 813 5 0.50-100 0.999 9 0.000 06 0.000 2
24 Ni60 C=0.284 332 1I-0.233 760 7 0.50-100 0.999 8 0.002 0.006
25 Pb208 C=0.039 093 5I-0.541 734 8 0.50-100 0.999 9 0.001 0.004
26 Pr141 C=0.029 440 0I+0.413 322 3 0.50-100 0.999 8 0.000 06 0.000 2
27 Rb85 C=0.594 836 4I+0.364 683 6 0.50-100 0.999 9 0.000 3 0.000 8
28 Sc45 C=1.183 274I+0.498 099 5 0.50-100 0.999 8 0.000 5 0.002
29 Sm147 C=0.093 714 1I+0.373 438 3 0.50-100 0.999 9 0.000 1 0.000 4
30 Sr88 C=0.250 044 5I+0.283 439 7 0.50-100 0.999 8 0.001 0.004
31 Tb159 C=0.017 194 5I+0.329 0511 0.50-100 0.999 8 0.000 2 0.000 7
32 Th232 C=0.027 729 3I+0.189 597 5 0.50-100 0.999 9 0.000 4 0.001
33 Tl205 C=0.027 957 4I-0.148 459 4 0.50-100 0.999 9 0.000 6 0.000 2
34 Tm169 C=0.020 832 4I+0.655 435 6 0.50-100 0.999 3 0.000 07 0.000 2
35 V51 C=0.382 192 9I+0.376 613 7 0.50-100 0.999 9 0.000 3 0.000 8
36 Y89 C=0.114 733 4I+0.318 146 4 0.50-100 0.999 9 0.000 1 0.000 4
37 Yb172 C=0.050 401 8I+0.049 465 6 0.50-100 0.999 9 0.000 3 0.000 9
), ArticleFig(id=1197097899109691865, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=EN, label=Tab.3, caption=

Recovery rate, precision and repeatability of 37 trace elements in samples. n=6

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Serial
number		 Element Recovery rate of labeled samples(RSD)/% Precision
RSD/%		 Repeatability
RSD/%
L2 RSD L4 RSD L6 RSD
1 Ag107 96.4 4.6 97.3 2.4 95.4 1.1 0.8 0.4
2 As75 88.3 1.3 86.8 1.5 84.5 0.9 0.6 1.8
3 Ba137 109 2.6 99.5 0.8 98.1 0.6 0.2 1.2
4 Be9 102 3.4 99.1 3.2 98.7 2.8 0.3 4.8
5 Bi209 103 3.8 95.4 2.1 98.1 1.0 1.1 0.6
6 Cd111 87.8 1.3 91.4 0.5 95.2 0.8 1.8 0.9
7 Ce140 98.3 1.8 96.7 0.9 97.1 1.2 0.4 1.1
8 Co59 99.9 1.3 97.7 1.0 98.7 0.6 0.3 1.1
9 Cr52 81.8 2.6 89.4 1.5 106 1.1 2.1 1.3
10 Cs133 97.8 1.4 97.8 0.9 96.5 0.5 0.6 1.4
11 Cu63 97.2 4.8 94.4 3.6 93.9 1.9 2.3 0.5
12 Dy163 109 1.5 103 0.6 106 1.2 0.3 1.1
13 Er166 109 1.2 101 0.6 107 0.5 0.2 0.9
14 Eu153 96.8 1.3 95.6 0.8 97.4 0.3 0.1 1.0
15 Gd157 95.6 0.9 98.9 1.0 97.6 0.4 0.2 0.9
16 Hg202 76.5 3.8 86.7 3.2 83.8 2.7 3.6 2.7
17 Ho165 108 1.1 104 1.3 107 0.8 0.4 0.6
18 In115 95.8 1.2 98.5 0.8 96.2 0.4 0.8 1.3
19 La139 93.5 2.7 93.6 1.9 95.9 0.7 0.2 1.0
20 Li7 110 4.2 88.5 3.3 84.7 2.9 1.6 3.5
21 Lu175 108 2.5 102 1.3 107 1.1 0.1 0.5
22 Mn55 102 3.9 96.7 3.7 93.8 2.1 1.5 1.3
23 Nd146 97.5 1.4 98.1 1.6 96.6 2.0 0.5 1.2
24 Ni60 89.1 2.8 90.3 1.7 87.7 1.1 1.8 1.0
25 Pb208 109 2.6 98.3 2.8 104 3.1 1.8 0.7
26 Pr141 96.6 1.1 98.5 1.5 97.4 0.5 0.7 1.1
27 Rb85 99.1 1.6 95.9 1.1 98.5 0.4 0.3 1.3
28 Sc45 103 1.3 106 0.8 103 0.9 0.4 1.9
29 Sm147 96.4 0.9 94.8 1.1 97.1 0.6 0.6 1.1
30 Sr88 104 3.3 97.6 3.8 98.6 1.5 1.4 1.3
31 Tb159 96.8 1.5 98.8 1.8 97.9 0.4 0.4 2.1
32 Th232 98.1 0.9 96.4 0.6 95.9 0.6 0.7 1.3
33 Tl205 104 0.9 102 1.1 104 0.5 0.3 1.0
34 Tm169 88.2 1.1 95.5 0.9 109 0.3 0.4 1.1
35 V51 102 2.4 99.6 0.5 102 1.2 0.5 1.0
36 Y89 102 1.2 95.8 1.3 104 0.8 0.3 1.1
37 Yb172 106 0.3 99.2 1.5 102 0.9 0.2 0.9
), ArticleFig(id=1197097899172606426, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=CN, label=表3, caption=

37种微量元素方法加标回收率、精密度、重复性. n=6

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Serial
number		 Element Recovery rate of labeled samples(RSD)/% Precision
RSD/%		 Repeatability
RSD/%
L2 RSD L4 RSD L6 RSD
1 Ag107 96.4 4.6 97.3 2.4 95.4 1.1 0.8 0.4
2 As75 88.3 1.3 86.8 1.5 84.5 0.9 0.6 1.8
3 Ba137 109 2.6 99.5 0.8 98.1 0.6 0.2 1.2
4 Be9 102 3.4 99.1 3.2 98.7 2.8 0.3 4.8
5 Bi209 103 3.8 95.4 2.1 98.1 1.0 1.1 0.6
6 Cd111 87.8 1.3 91.4 0.5 95.2 0.8 1.8 0.9
7 Ce140 98.3 1.8 96.7 0.9 97.1 1.2 0.4 1.1
8 Co59 99.9 1.3 97.7 1.0 98.7 0.6 0.3 1.1
9 Cr52 81.8 2.6 89.4 1.5 106 1.1 2.1 1.3
10 Cs133 97.8 1.4 97.8 0.9 96.5 0.5 0.6 1.4
11 Cu63 97.2 4.8 94.4 3.6 93.9 1.9 2.3 0.5
12 Dy163 109 1.5 103 0.6 106 1.2 0.3 1.1
13 Er166 109 1.2 101 0.6 107 0.5 0.2 0.9
14 Eu153 96.8 1.3 95.6 0.8 97.4 0.3 0.1 1.0
15 Gd157 95.6 0.9 98.9 1.0 97.6 0.4 0.2 0.9
16 Hg202 76.5 3.8 86.7 3.2 83.8 2.7 3.6 2.7
17 Ho165 108 1.1 104 1.3 107 0.8 0.4 0.6
18 In115 95.8 1.2 98.5 0.8 96.2 0.4 0.8 1.3
19 La139 93.5 2.7 93.6 1.9 95.9 0.7 0.2 1.0
20 Li7 110 4.2 88.5 3.3 84.7 2.9 1.6 3.5
21 Lu175 108 2.5 102 1.3 107 1.1 0.1 0.5
22 Mn55 102 3.9 96.7 3.7 93.8 2.1 1.5 1.3
23 Nd146 97.5 1.4 98.1 1.6 96.6 2.0 0.5 1.2
24 Ni60 89.1 2.8 90.3 1.7 87.7 1.1 1.8 1.0
25 Pb208 109 2.6 98.3 2.8 104 3.1 1.8 0.7
26 Pr141 96.6 1.1 98.5 1.5 97.4 0.5 0.7 1.1
27 Rb85 99.1 1.6 95.9 1.1 98.5 0.4 0.3 1.3
28 Sc45 103 1.3 106 0.8 103 0.9 0.4 1.9
29 Sm147 96.4 0.9 94.8 1.1 97.1 0.6 0.6 1.1
30 Sr88 104 3.3 97.6 3.8 98.6 1.5 1.4 1.3
31 Tb159 96.8 1.5 98.8 1.8 97.9 0.4 0.4 2.1
32 Th232 98.1 0.9 96.4 0.6 95.9 0.6 0.7 1.3
33 Tl205 104 0.9 102 1.1 104 0.5 0.3 1.0
34 Tm169 88.2 1.1 95.5 0.9 109 0.3 0.4 1.1
35 V51 102 2.4 99.6 0.5 102 1.2 0.5 1.0
36 Y89 102 1.2 95.8 1.3 104 0.8 0.3 1.1
37 Yb172 106 0.3 99.2 1.5 102 0.9 0.2 0.9
), ArticleFig(id=1197097899243909595, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195664140745356284, language=EN, label=Tab.4, caption=

Contents of 37 elements in 40 batches of cistanches herba

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Element Content/mg·kg-1 Detection
rate/%
S1 S2 S3 S4 S5 S6 S7 S8 S9 S10 S11 S12 S13 S14 S15 S16 S17 S18 S19 S20
Ag ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
As ND ND 7.5 ND ND ND ND ND ND ND ND 0.4 0.1 ND 0.4 ND ND ND ND ND 7.5
Ba 2.9 0.9 100 1.8 2.8 2.3 2.6 1.7 1.0 4.1 1.3 16.8 35.7 8.0 42.4 18.3 2.7 5.4 1.1 1.5 100
Be ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Bi ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cd ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Ce ND ND 25 ND ND ND ND ND ND 1.2 1.4 1.5 1.1 0.5 2.0 0.7 0.7 0.8 ND ND 25
Co ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cr 5.2 1.4 100 3.5 2.5 2.3 2.7 1.0 0.8 6.7 1.2 7.8 9.9 1.6 19.0 5.3 5.1 3.1 2.0 2.0 100
Cs ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cu 5.4 0.7 100 1.0 5.7 4.2 9.2 5.8 5.8 5.6 5.6 3.2 8.8 2.0 7.2 4.1 2.0 5.8 5.8 6.7 100
Dy ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Er ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Eu ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Gd ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Hg 0.1 0.2 82.5 0.1 ND ND ND ND ND ND ND 0.1 0.2 0.1 0.1 0.1 0.1 0.1 0.1 0.1 82.5
Ho ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
In ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
La ND ND 2.5 ND ND ND ND ND ND ND ND ND ND ND 1.1 ND ND ND ND ND 2.5
Li ND ND 42.5 ND 1.5 1.2 ND ND 2.2 0.5 ND 1.1 1.1 0.6 2.6 1.9 1.3 1.3 1.9 ND 42.5
Lu ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Mn 13.6 1.9 100 4.3 5.5 4.6 4.4 3.3 28.6 45.8 58.3 2.9 8.3 13.2 3.1 6.4 25.0 13.1 2.9 2.8 100
Nd ND ND 12.5 ND ND ND ND ND ND ND 1.0 1.1 0.8 0.5 1.4 ND ND ND ND ND 12.5
Ni 1.6 0.5 100 0.8 1.5 3.9 2.4 1.9 1.8 2.9 1.9 3.9 2.8 1.4 5.3 1.5 1.6 2.3 1.0 0.7 100
Pb ND ND 27.5 ND ND ND ND ND ND ND ND 0.4 0.2 ND 0.7 0.0 0.5 0.2 ND ND 27.5
Pr ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Rb 30.3 1.4 100 1.7 4.5 4.9 4.2 2.9 3.7 4.8 3.4 28.5 31.2 21.7 12.7 16.9 6.0 5.6 6.3 3.0 100
Sc ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sm ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sr 26.3 3.9 100 5.4 12.9 14.3 12.2 6.3 9.4 14.4 8.5 65.3 106.7 69.1 110.8 57.2 16.0 4.9 19.3 9.1 100
Tb ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Th ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tl ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tm ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
V ND ND 20 ND ND ND ND ND ND 1.0 ND 2.2 1.8 0.9 3.0 1.1 0.8 1.0 ND ND 20
Y ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Yb ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Element Content/mg·kg-1 Detection
rate/%
S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34 S35 S36 S37 S38 S39 S40
Ag ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
As ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 7.5
Ba 2.0 0.8 1.1 1.8 2.0 6.9 2.2 1.6 3.6 1.7 3.7 4.3 2.4 0.3 0.9 0.4 0.8 0.4 3.1 1.0 100
Be ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Bi ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cd ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Ce ND ND ND ND ND 1.2 ND ND ND ND ND ND ND ND ND ND ND ND ND ND 25
Co ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cr 1.9 0.7 2.0 2.2 3.6 4.7 1.9 1.3 2.9 2.8 5.3 9.3 1.0 0.5 2.3 0.8 1.3 2.9 0.8 0.4 100
Cs ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cu 8.4 6.3 4.9 6.4 5.8 9.6 7.0 5.6 7.1 9.7 8.4 10.6 4.5 3.5 5.2 5.7 3.9 5.7 6.6 4.2 100
Dy ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Er ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Eu ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Gd ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Hg 0.1 0.2 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.2 0.1 0.1 0.1 0.1 0.2 0.1 0.1 82.5
Ho ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
In ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Element Content/mg·kg-1 Detection
rate/%
S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34 S35 S36 S37 S38 S39 S40
La ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 2.5
Li ND ND 4.5 ND ND ND ND ND 6.0 0.4 1.1 ND ND ND ND ND ND ND ND 2.6 42.5
Lu ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Mn 4.3 11.8 3.5 5.1 11.9 16.8 6.0 11.0 5.8 10.6 6.6 13.0 3.2 1.2 11.3 11.8 1.9 3.5 28.8 1.5 100
Nd ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 12.5
Ni 1.3 0.6 0.6 2.0 1.4 3.3 1.7 1.6 1.2 2.4 1.4 3.3 0.7 0.2 1.6 1.2 0.5 0.8 2.4 0.3 100
Pb ND ND ND ND ND 0.2 ND ND 0.2 0.1 0.2 0.1 ND ND ND ND ND ND ND ND 27.5
Pr ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Rb 5.2 3.0 5.1 3.6 5.2 7.7 11.2 7.0 8.2 3.9 3.1 13.0 2.5 3.2 5.0 7.9 2.9 4.4 4.4 2.8 100
Sc ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sm ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sr 10.0 7.0 10.9 6.6 9.3 13.3 8.8 7.9 12.0 3.4 8.0 8.1 4.0 6.6 10.3 2.8 4.9 10.2 8.8 3.9 100
Tb ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Th ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tl ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tm ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
V ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 20
Y ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Yb ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
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40批肉苁蓉中37种元素的含量

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Element Content/mg·kg-1 Detection
rate/%
S1 S2 S3 S4 S5 S6 S7 S8 S9 S10 S11 S12 S13 S14 S15 S16 S17 S18 S19 S20
Ag ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
As ND ND 7.5 ND ND ND ND ND ND ND ND 0.4 0.1 ND 0.4 ND ND ND ND ND 7.5
Ba 2.9 0.9 100 1.8 2.8 2.3 2.6 1.7 1.0 4.1 1.3 16.8 35.7 8.0 42.4 18.3 2.7 5.4 1.1 1.5 100
Be ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Bi ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cd ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Ce ND ND 25 ND ND ND ND ND ND 1.2 1.4 1.5 1.1 0.5 2.0 0.7 0.7 0.8 ND ND 25
Co ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cr 5.2 1.4 100 3.5 2.5 2.3 2.7 1.0 0.8 6.7 1.2 7.8 9.9 1.6 19.0 5.3 5.1 3.1 2.0 2.0 100
Cs ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cu 5.4 0.7 100 1.0 5.7 4.2 9.2 5.8 5.8 5.6 5.6 3.2 8.8 2.0 7.2 4.1 2.0 5.8 5.8 6.7 100
Dy ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Er ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Eu ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Gd ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Hg 0.1 0.2 82.5 0.1 ND ND ND ND ND ND ND 0.1 0.2 0.1 0.1 0.1 0.1 0.1 0.1 0.1 82.5
Ho ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
In ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
La ND ND 2.5 ND ND ND ND ND ND ND ND ND ND ND 1.1 ND ND ND ND ND 2.5
Li ND ND 42.5 ND 1.5 1.2 ND ND 2.2 0.5 ND 1.1 1.1 0.6 2.6 1.9 1.3 1.3 1.9 ND 42.5
Lu ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Mn 13.6 1.9 100 4.3 5.5 4.6 4.4 3.3 28.6 45.8 58.3 2.9 8.3 13.2 3.1 6.4 25.0 13.1 2.9 2.8 100
Nd ND ND 12.5 ND ND ND ND ND ND ND 1.0 1.1 0.8 0.5 1.4 ND ND ND ND ND 12.5
Ni 1.6 0.5 100 0.8 1.5 3.9 2.4 1.9 1.8 2.9 1.9 3.9 2.8 1.4 5.3 1.5 1.6 2.3 1.0 0.7 100
Pb ND ND 27.5 ND ND ND ND ND ND ND ND 0.4 0.2 ND 0.7 0.0 0.5 0.2 ND ND 27.5
Pr ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Rb 30.3 1.4 100 1.7 4.5 4.9 4.2 2.9 3.7 4.8 3.4 28.5 31.2 21.7 12.7 16.9 6.0 5.6 6.3 3.0 100
Sc ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sm ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sr 26.3 3.9 100 5.4 12.9 14.3 12.2 6.3 9.4 14.4 8.5 65.3 106.7 69.1 110.8 57.2 16.0 4.9 19.3 9.1 100
Tb ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Th ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tl ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tm ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
V ND ND 20 ND ND ND ND ND ND 1.0 ND 2.2 1.8 0.9 3.0 1.1 0.8 1.0 ND ND 20
Y ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Yb ND ND 0 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Element Content/mg·kg-1 Detection
rate/%
S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34 S35 S36 S37 S38 S39 S40
Ag ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
As ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 7.5
Ba 2.0 0.8 1.1 1.8 2.0 6.9 2.2 1.6 3.6 1.7 3.7 4.3 2.4 0.3 0.9 0.4 0.8 0.4 3.1 1.0 100
Be ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Bi ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cd ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Ce ND ND ND ND ND 1.2 ND ND ND ND ND ND ND ND ND ND ND ND ND ND 25
Co ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cr 1.9 0.7 2.0 2.2 3.6 4.7 1.9 1.3 2.9 2.8 5.3 9.3 1.0 0.5 2.3 0.8 1.3 2.9 0.8 0.4 100
Cs ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Cu 8.4 6.3 4.9 6.4 5.8 9.6 7.0 5.6 7.1 9.7 8.4 10.6 4.5 3.5 5.2 5.7 3.9 5.7 6.6 4.2 100
Dy ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Er ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Eu ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Gd ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Hg 0.1 0.2 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.2 0.1 0.1 0.1 0.1 0.2 0.1 0.1 82.5
Ho ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
In ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Element Content/mg·kg-1 Detection
rate/%
S21 S22 S23 S24 S25 S26 S27 S28 S29 S30 S31 S32 S33 S34 S35 S36 S37 S38 S39 S40
La ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 2.5
Li ND ND 4.5 ND ND ND ND ND 6.0 0.4 1.1 ND ND ND ND ND ND ND ND 2.6 42.5
Lu ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Mn 4.3 11.8 3.5 5.1 11.9 16.8 6.0 11.0 5.8 10.6 6.6 13.0 3.2 1.2 11.3 11.8 1.9 3.5 28.8 1.5 100
Nd ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 12.5
Ni 1.3 0.6 0.6 2.0 1.4 3.3 1.7 1.6 1.2 2.4 1.4 3.3 0.7 0.2 1.6 1.2 0.5 0.8 2.4 0.3 100
Pb ND ND ND ND ND 0.2 ND ND 0.2 0.1 0.2 0.1 ND ND ND ND ND ND ND ND 27.5
Pr ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Rb 5.2 3.0 5.1 3.6 5.2 7.7 11.2 7.0 8.2 3.9 3.1 13.0 2.5 3.2 5.0 7.9 2.9 4.4 4.4 2.8 100
Sc ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sm ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Sr 10.0 7.0 10.9 6.6 9.3 13.3 8.8 7.9 12.0 3.4 8.0 8.1 4.0 6.6 10.3 2.8 4.9 10.2 8.8 3.9 100
Tb ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Th ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tl ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Tm ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
V ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 20
Y ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
Yb ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0
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ICP-MS测定不同产地肉苁蓉中多种微量元素的含量
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徐勤科 , 魏学冰 , 李莉 , 尉鹏 , 郭朝晖 , 孙莺 *
中国药学杂志 | 论著 2024,59(2): 179-185
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中国药学杂志 | 论著 2024, 59(2): 179-185
ICP-MS测定不同产地肉苁蓉中多种微量元素的含量
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徐勤科, 魏学冰, 李莉, 尉鹏, 郭朝晖, 孙莺*
作者信息
  • 甘肃省药品检验研究院, 兰州 730000

    • 徐勤科,男,硕士,高级工程师 研究方向:药品质量控制及标准研究

通讯作者:

*孙莺,女,博士,主任药师 研究方向:药品质量控制 Tel:(0931)7822939
Determination of Trace Elements in Cistanches Herba from Different Habitats by ICP-MS
XU Qinke, WEI Xuebing, LI Li, WEI Peng, GUO Zhaohui, SUN Ying*
Affiliations
  • Gansu Pharmaceutical Inspection Institute, Lanzhou 730000, China
出版时间: 2024-01-22 doi: 10.11669/cpj.2024.02.010
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摘要
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目的 建立37种元素的微波消解-电感耦合等离子体质谱(ICP-MS)测定方法,并对不同产地的肉苁蓉中37种无机元素进行检测分析,初步探索研究不同产地肉苁蓉中多种无机元素的污染分布情况。方法 以硝酸-过氧化氢为消解试剂,采用微波消解法对样品进行前处理,通过采用在线内标校正,外标法定量ICP-MS 法同时测定肉苁蓉中37种无机元素的含量。结果 在曲线范围0.50~100 μg·L-1(Hg:0.20~20 μg·L-1)内与峰面积呈良好的线性关系(r≥0.997 4),检出限为0.000 27~0.045 μg·L-1,加标回收率在高、中、低3 个添加水平下,元素的平均回收率介于76.5%~110.0%,仪器精密度和重复性的相对标准偏差(RSD)值均<4.8%;40批肉苁蓉中5种《中国药典》2020年版明确需要控制的有害重金属元素(铜、铅、砷、汞、镉)的检出率分别为27.5%、7.5%、82.5%、0和100%;钡元素、锰元素、铷元素和锶元素在 40 批样品检出率均为100%,且含量远远高于其他元素,具有明显的地域性差异。结论 该方法灵敏度高、重现性好、缩短了检验时间、降低了检验成本,可同时检测肉苁蓉中多种无机元素,为肉苁蓉的优化培育和保证药材品质以及用药安全提供数据支撑。

肉苁蓉  /  无机元素  /  微波消解  /  电感耦合等离子体质谱法

OBJECTIVE To establish a method for the determination of 37 kinds of inorganic elements by microwave digestion and inductively coupled plasma mass spectrometer (ICP-MS), and to detect and analyze 37 kinds of inorganic elements in cistanches herba from different habitats, and to preliminatively explore the pollution distribution of various inorganic elements in cistanches herba from different habitats. METHODS Using nitric acid and hydrogen peroxide as digestion reagent, microwave digestion was used to pretreat the samples. The contents of 37 inorganic elements in cistanches herba were determined simultaneously by internal standard correction and external standard quantitative ICP-MS method. RESULTS In the curve range of 0.50-100 μg·L-1(Hg: 0.20-20 μg·L-1) showed a good linear relationship with the peak area (r≥0.997 4). The detection limits were 0.000 27-0.045 μg·L-1. The average recoveries were 76.5% to 110.0% at high, medium and low levels. RSD of precision and repeatability were lower than 4.8%. The detection rates of 5 harmful heavy metal elements (copper, lead, arsenic, mercury, cadmium) that need to be controlled by Chinese Pharmacopoeia (2015 edition) in 40 batches of cistanches herba were 27.5%, 7.5%, 82.5%, 0 and 100%, respectively. The detection rate of barium, manganese, rubidium and strontium in 40 batches of samples is 100%, and the content is much higher than other elements,there are obvious regional differences. CONCLUSION This method has high sensitivity, good reproducibility, reduced the inspection time and cost, and can simultaneously detect various inorganic elements in cistanches herba, providing data support for optimal cultivation, quality assurance and drug safety of cistanches herba.

cistanches herba  /  inorganic element  /  microwave digestion  /  ICP-MS
徐勤科, 魏学冰, 李莉, 尉鹏, 郭朝晖, 孙莺. ICP-MS测定不同产地肉苁蓉中多种微量元素的含量. 中国药学杂志, 2024 , 59 (2) : 179 -185 . DOI: 10.11669/cpj.2024.02.010
XU Qinke, WEI Xuebing, LI Li, WEI Peng, GUO Zhaohui, SUN Ying. Determination of Trace Elements in Cistanches Herba from Different Habitats by ICP-MS[J]. Chinese Pharmaceutical Journal, 2024 , 59 (2) : 179 -185 . DOI: 10.11669/cpj.2024.02.010
正文
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肉苁蓉属(Cistanche)植物为列当科(Orobanchaceae)多年生专性根全寄生植物,又名大芸、地精、金笋等[1]。我国有肉苁蓉属植物 4 种 1 变种,包括荒漠肉苁蓉、管花肉苁蓉、盐生肉苁蓉、白花盐苁蓉以及沙苁蓉。《中国药典》2020年版收载的肉苁蓉为荒漠肉苁蓉和管花肉苁蓉的干燥肉质茎。管花肉苁蓉寄生于沙漠柽柳属根部,主要分布在新疆南疆沙漠地区。荒漠肉苁蓉寄生于固沙防风植物梭梭树的根部,主要分布于内蒙古地区的阿拉善盟(左旗、右旗、额济纳旗)、甘肃和新疆北部等沙漠地区[2-7]。
无机元素在植物的整个生长周期起着重要的作用,由于地域及生长环境的影响,在植物体中的无机元素残留量也有所不同,而对人体来说,当其处于最适宜浓度范围内时人体才会处于健康状态。有些无机元素属于外源性有害元素,例如铅、镉、铬、砷和汞等无机金属是中药的重要污染物;还有一些虽然是人体必需的微量元素,如铜、铁、锌等,但是在人体内蓄积到一定浓度时就会破坏平衡从而产生病变[8-9]。肉苁蓉既是药材又可以作为食材,所以它的无机元素的蓄积应该引起关注,有必要对其多种无机元素的含量进行检测分析。笔者依据《中国药典》通用指导原则采用微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定肉苁蓉中37 种无机元素,通过检验检测的数据统计分析,从而为肉苁蓉的优化培育和品质保证以及用药安全提供数据支撑。
1 试剂与仪器
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1.1 仪器
岛津2030电感耦合等离子体质谱仪(日本岛津公司);Multiwate 7000微波消解仪 (奥地利安东帕公司);ME204电子天平(瑞士梅特勒公司)。Milli-Q超纯水仪(美国Millipore公司)。
1.2 试剂
锂等36 种元素混标标准溶液(质量浓度为10 μg·mL-1);汞单元素标准溶液(质量浓度为1 000 μg·mL-1);铼(Re)内标溶液(质量浓度为1 000 μg·mL-1);铑(Rh)内标溶液(质量浓度为1 000 μg·mL-1,安捷伦公司);超纯水(电阻率18.2 MΩ·cm)实验室自制;硝酸(68.0%~70.0%,UPS级)、过氧化氢(30.0%~32.0%,UPS级)(苏州晶瑞化学股份有限公司)。
1.3 试验样品
40批次肉苁蓉药材及饮片收集于各药材生产企业、零售药店及自采,产地分别来自新疆、甘肃和内蒙古,经甘肃省药品检验研究院宋平顺主任药师鉴定为正品,收集的样品经手工除去泥沙等杂质后晾干,备用。
2 方法与结果
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2.1 标准储备溶液的制备
精密量取锂等36种元素混合标准品溶液(10 mg·L-1)适量,用体积分数2%硝酸水溶液稀释配制得到质量浓度为1 000 μg·L-1的锂等36种元素混合标准储备液,并保存于-5 ℃低温冰箱中;精密量取汞单元素标准品溶液(1 000 mg·L-1)适量,加体积分数2%硝酸水溶液稀释配制得到质量浓度为100 μg·L-1汞单元素标准储备液,需现用现配。
2.2 内标溶液的制备
精密量取Re内标溶液和Rh内标溶液适量,加体积分数2%硝酸水溶液稀释配制得到质量浓度为500 μg·L-1的混合内标使用溶液。
2.3 供试品溶液的制备
精密称取肉苁蓉样品粉末(过3号筛)约0.3 g置于消解罐中,加入2 mL硝酸和1 mL的超纯水,静置过夜,次日再加入1 mL过氧化氢置于微波消解炉内消解(消解程序见表1),消解完成后,取出消解罐置于电加热板上(温度低于100 ℃)缓慢加热,待消解罐内红棕色蒸汽挥尽即可取出放冷至室温,消解液用超纯水分多次转移至50 mL量瓶中,用超纯水定容至刻度,同法做样品空白,供ICP-MS测定。
2.4 ICP-MS工作条件
射频功率1 550 W,雾化室温度5 ℃,为碰撞反应模式,采样深度5.0 mm,等离子体氩气流速11.0 L·min-1,雾化器氩气流速0.7 L·min-1,测量元素积分时间分割次数10次,同一样品测量3 次求其平均值。分析过程中,为校正补偿样品的基体效应和信号漂移,对所测定元素不产生干扰的情况下选择Re和Rh作为在线内标。
2.5 线性范围、检出限和定量限
分别精密量取锂等36种混合标准储备液0.05、0.1、0.5、1.0、5.0、10.0 mL和汞单元素标准储备液0.20、0.50、1.0、2.0、5.0、20.0 mL于100 mL量瓶中,加2%硝酸溶液稀释至刻度,摇匀。配制成0.50、1.0、5.0、10.0、50.0、100.0 μg·L-1的锂等36种混合标准系列溶液和0.20、0.50、1.0、2.0、5.0、20.0 μg·L-1的汞单元素标准系列溶液,临用现制。
调节ICP-MS至最佳工作状态,测定已配制好的标准曲线溶液,以其响应值对其质量浓度进行线性回归,得到线性方程。结果表明,测定元素的响应值在质量浓度 0.50~100 μg·L-1(Hg:0.20~20 μg·L-1)范围内线性关系良好,相关系数均大于0.997 4,表明在该质量浓度范围内,所测定元素的仪器响应与其质量浓度是线性的。检出限和定量限均由仪器做完标准曲线后仪器自动给出,结果见表2。
2.6 加标回收率
为了验证此方法的准确性和可靠性,对样品进行了加标测定,加标分为高、中、低3种浓度添加。加标方法为:精密称取已知含量的肉苁蓉样品18份,分别精密加入混合标准系列溶液的第二个浓度点(L2)、第四个浓度点(L4)和第六个浓度点(L6)适量,每个浓度点制备6份,按试验方法进行前处理和检测,每个样品平行测定 3 次,取其平均值计算回收率。37种元素的回收率均在 76.5%~110.0%之间,内标RSD均小于5.0%,表明本实验方法可靠。实验结果见表3。
2.7 重复性试验
随机选取肉苁蓉样品一批,准确称取样品,样品的前处理方法制备,平行 6 份,按“2.4”项下仪器条件进行测定。计算RSD值均在0.4%~4.8%,表明该试验重复性良好,结果见表3。
2.8 进样精密度试验
取“2.5”项下配制的混合标准系列溶液中间的浓度点(质量浓度10 μg·L-1),连续进样 6 次,计算相对标准偏差(RSD)值均在 0.1%~3.6%,表明该试验精密度良好,结果见表3。
2.9 基质对检测信号强度的影响
取制备好的肉苁蓉样品溶液6批次以及试剂空白分别进样6 次,筛选样品中均未检出的元素与试剂空白对应的元素比较其信号强度,发现样品基质对检测信号强度基本没有影响。
2.10 样品测定
取肉苁蓉样品,按供试品溶液制备方法制备,在ICP-MS工作条件下测定样品中的 37 种无机元素,结果见表4。结果显示,40 批肉苁蓉中金属元素及有害元素铅、砷、汞、镉和铜的检出率分别为27.5%、7.5%、82.5%、0和100%。由此可见,肉苁蓉中重金属元素的检出情况较好。另外,钡元素、铬元素、锰元素、镍元素、铷元素和锶元素在 40 批样品检出率均为 100%,钡元素的含量为0.3~42.4 mg·kg-1,铬元素的含量为0.4~19.0 mg·kg-1,锰元素的含量为01.2~58.3 mg·kg-1,镍元素的含量为0.2~5.3 mg·kg-1,铷元素的含量为1.4~31.2 mg·kg-1,锶元素的含量为2.8~110.8 mg·kg-1,锰和锶的最大含量远高于其他元素,需引起关注。
3 讨论
收起
待测物在ICP-MS的检测过程中,前处理对于结果的准确性非常重要,前处理过程需要样品完全溶解到消解液中,只有样品完全溶解到消解液时的供试品溶液才是澄清透明的。该研究采用超级微波消解仪,相比较于传统的微波消解仪可以达到更高的温度、更高的压力并且同时可以在相同的温度和压力下处理更多的样品。这样的优势下,样品在处理过程中加入的酸就相对更少,使得样品在消解完成后不需要赶酸过程,缩短前处理时间,可以直接进行ICP-MS的检测,较少的酸加入量可以提升仪器使用寿命、降低试验人员安全风险以及减少对环境的污染。
在ICP-MS的检测过程中,在质量数的选择过程中,一般推荐所测元素所有质量数中,占比最高的首选,但是在实际测定过程中,镉(Cd114)和镍(Ni58)都是所在元素质量数占比最高的,而这两个元素都有严重的干扰问题,加标回收率达不到要求,所以该试验选取了Cd111和Ni60作为检测对象。
《中国药典》2015年版中规定了重金属及有害元素含量的有17 种药材,元素含量为铅≤5 mg·kg-1;镉≤0.3 mg·kg-1;砷≤2 mg·kg-1;汞≤0.2 mg·kg-1;铜≤20 mg·kg-1,肉苁蓉未列入其中,但重金属及有害元素含量可参考其标准限量,样品结果表明,这 5 种重金属及有害元素均在限度范围内。
肉苁蓉基于生长的特殊性,主产地主要有新疆、甘肃和内蒙古,本研究主要分析了无机元素检出率均为100%的钡元素、铬元素、锰元素、镍元素、铷元素和锶元素,其中铬元素和镍元素最大含量和均值含量3大产地均在同一数量级,说明没有明显的地域差别。但是产地新疆的钡元素和锶元素含量最大值分别为42.4 mg·kg-1和110.8 mg·kg-1,产地甘肃的锰元素含量最大值为58.3 mg·kg-1,产地内蒙古的铷元素含量最大值为31.3 mg·kg-1,说明肉苁蓉中钡元素、锶元素、锰元素和铷元素有明显的地域性差异。
无机元素对于人体有必须微量元素和非必需微量元素,而在ICH元素指导原则中将重金属元素分为三类,第一类包括铅、砷、汞、镉具有明显的毒性,需要进行风险评估;第二类元素如果是刻意添加或者给药途径不同时也需要进行风险评估,包括钒、钴、铊、银、锑、钡、锂、铬、铜、锡、镍等;第三类元素为没有明显的毒性元素,没有明确规定需要进行安全评价的元素。肉苁蓉中含量较高且检出率高的钡和铷都是人体非必需元素,铬、锰、镍和锶都是人体必需微量元素。微量元素在人体中需要保持一种动态平衡,摄入过多或过少都会对身体健康产生影响,而且钡、铬、镍元素在特定的用药环境下均需做安全评价的。例如,铬元素的主要功能是三价铬使胰岛素发挥正常功能,但铬元素摄入过多三价铬会转变为六价铬,六价铬有很强的毒性会导致人体各种病变甚至癌变[10-13]。因此肉苁蓉中除药典规定的重金属元素的含量外,其他元素的含量也应引起重视。
4 结论
收起
本研究通过微波消解-电感耦合等离子体质谱法对肉苁蓉中37种无机元素进行了定量分析,建立了肉苁蓉中37种无机元素的测定方法。该方法具有简便、快速、准确的优点,可用于肉苁蓉中 37 种无机元素的含量测定。
基金
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  • 2020年中药材及饮片质量控制重点实验室项目资助(2020GSMPA-KL08)
文献
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2024年第59卷第2期
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doi: 10.11669/cpj.2024.02.010
  • 接收时间：2023-05-31
  • 首发时间：2025-11-13
  • 出版时间：2024-01-22
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  • 收稿日期：2023-05-31
基金
2020年中药材及饮片质量控制重点实验室项目资助(2020GSMPA-KL08)
作者信息
    甘肃省药品检验研究院, 兰州 730000

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*孙莺,女,博士,主任药师 研究方向:药品质量控制 Tel:(0931)7822939
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2种不同金属材料的力学参数
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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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