Article(id=1292135430594515761, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1292135402790482407, articleNumber=null, orderNo=null, doi=10.13699/j.cnki.1001-6821.2026.11.013, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1774454400000, receivedDateStr=2026-03-26, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1785998693369, onlineDateStr=2026-08-06, pubDate=1781625600000, pubDateStr=2026-06-17, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1785998693369, onlineIssueDateStr=2026-08-06, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1785998693369, creator=13701087609, updateTime=1785998693369, updator=13701087609, issue=Issue{id=1292135402790482407, tenantId=1146029695717560320, journalId=1246415772164075586, year='2026', volume='42', issue='11', pageStart='1501', pageEnd='1650', issueExtLink='null', onlineDate='null', pubDate='1781625600000', pubDateStr='2026-06-17', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1785998686739, creator='13701087609', updateTime=1786014315540, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1292200954833686587, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1292135402790482407, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1292200954833686588, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1292135402790482407, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1581, endPage=1585, ext={EN=ArticleExt(id=1292135430997168946, articleId=1292135430594515761, tenantId=1146029695717560320, journalId=1246415772164075586, language=EN, title=Determination of salmon calcitonin concentration in human plasma by HPLC-MS/MS method, columnId=1246531413395263850, journalTitle=Chinese Journal of Clinical Pharmacology, columnName=Research Method, runingTitle=null, highlight=null, articleAbstract=
Objective

To establish a high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of calcitonin salmon in human plasma.

Method

Precipitate plasma samples using organic reagents, then centrifuge and collect the supernatant, proceed with concentration, reconstitution, and sample injection, and a phenomenex Jupiter® C4-300A column (2.1 mm×50.0 mm, 5.0 μm) was used for chromatographic separation. The mobile phase was 0.1% formic acid water (phase A) -0.1% formic acid acetonitrile (phase B); gradient elution with a flow rate of 0.50 mL·min-1, column temperature 50 ℃, injection volume 20 μL. A custom-labeled isotopic compound was used as the internal standard, scanning was carried out by means of multi reaction monitoring (MRM) in the positive ionization mode with an electric spray ionization source(ESI). Examine the specificity, standard curve, lower limit of quantification (LLOQ), precision, accuracy, recovery rate, matrix effect, and stability of the method.

Result

The method showed a good specificity results of the method, and there is no interference between the analyte and the internal standard. The linear range of the standard curves for the tested substances was 2.00、4.00、10.00、50.00、100.00、200.00、360.00、400.00 pg·mL-1, The standard curve was y=2.98×10-2x+5.30×10-3 (R2=0.997 4) and the lower limit of quantification(LLOQ) is 2.00 pg·mL-1. The intra-day and inter day relative standard deviation (RSD) were both less than 15%, extraction recovery rates ranging from 60.13% to 75.39% (RSD<15%), and matrix effects ranging from 97.45% to 109.72% (RSD<10%). The stability of the matrix samples was verified by placing them at room temperature for 24 hours, repeatedly freezing and thawing at -20 ℃ and -70 ℃ for 5 times, freezing at -20 ℃ and -70 ℃ for 49 days, and placing the processed samples in an automatic sampler for 333 hours, with accuracy ranging from 97.03% to 108.64%, all stable.

Conclusion

The established HPLC-MS/MS method is simple, rapid, highly sensitive, and specific, and can be used for the detection of plasma samples in pharmacokinetic studies.

, authors=Xue-yi CHEN1, 2, Xiao-xia JU2, Ying WANG2, Xian-feng SHI2, Hong SHEN2, Lan-lan CAI2, Xiu-yan WEI1, authorsList=Xue-yi CHEN, Xiao-xia JU, Ying WANG, Xian-feng SHI, Hong SHEN, Lan-lan CAI, Xiu-yan WEI, authorCompany=null, correspAuthors=Xiu-yan WEI, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1292135431471125299, articleId=1292135430594515761, tenantId=1146029695717560320, journalId=1246415772164075586, language=CN, title=用HPLC-MS/MS法测定人血浆中鲑降钙素的浓度, columnId=1246531413600784769, journalTitle=中国临床药理学杂志, columnName=研究方法, runingTitle=null, highlight=null, articleAbstract=
目的

建立测定鲑降钙素血药浓度的高效液相色谱串联质谱(HPLC-MS/MS)方法。

方法

用有机试剂沉淀血浆样品,离心分离取上清,再进行浓缩、复溶、进样,用phenomenex Jupiter® C4-300A色谱柱(2.1 mm×50.0 mm,5.0 μm)进行色谱分离,流动相为0.1%甲酸水(A)-0.1%甲酸乙腈(B);梯度洗脱,流速为0. 50 mL·min-1,柱温为50 ℃,进样量为20 μL。以定制的同位素化合物为内标,用电喷雾电离源,用正电离模式,以多反应监测的方式进行扫描。考察该方法的专属性、标准曲线、定量下限、精密度、准确度、回收率、基质效应和稳定性。

结果

方法的专属性结果良好,待测物与内标之间相互无干扰,鲑降钙素的标准曲线线性范围为2.00、4.00、10.00、50.00、100.00、200.00、360.00、400.00 pg·mL-1,标准曲线为y=2.98×10-2x+5.30×10-3R2=0.997 4),定量下限为2.00 pg·mL-1。日内、日间相对标准偏差(RSD)均小于15%,提取回收率为60.13%~75.39%(RSD<15%),基质效应为97.45%~109.72%(RSD<10%)。基质样品在实验台室温放置24 h、在-20 ℃和-70 ℃下反复冻融进行5次、在-20 ℃和-70 ℃冻存49 d以及处理后样品在自动进样器中放置333 h的稳定性经验证,准确度在97.03%~108.64%,均稳定。

结论

本研究建立的HPLC-MS/MS方法简单、快速、灵敏度高、专属性好,可用于药代动力学研究中血浆样本的检测。

, authors=陈学义1, 2, 举晓霞2, 王颖2, 石先凤2, 沈虹2, 蔡兰兰2, 魏秀岩1, authorsList=陈学义, 举晓霞, 王颖, 石先凤, 沈虹, 蔡兰兰, 魏秀岩, authorCompany=null, correspAuthors=魏秀岩, authorNote=

陈学义(1992-),男,本科,初级药师,主要从事临床药代动力学生物样品分析方面的研究和工作

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魏秀岩,副教授,硕士生导师 MP: 13194225280 E-mail:
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用HPLC-MS/MS法测定人血浆中鲑降钙素的浓度
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陈学义 1, 2 , 举晓霞 2 , 王颖 2 , 石先凤 2 , 沈虹 2 , 蔡兰兰 2 , 魏秀岩 1
中国临床药理学杂志 | 研究方法 2026,42(11): 1581-1585
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中国临床药理学杂志 |研究方法 2026 , 42 (11) : 1581 -1585
用HPLC-MS/MS法测定人血浆中鲑降钙素的浓度
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陈学义(1992-),男,本科,初级药师,主要从事临床药代动力学生物样品分析方面的研究和工作

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陈学义(1992-),男,本科,初级药师,主要从事临床药代动力学生物样品分析方面的研究和工作

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陈学义1, 2, 举晓霞2, 王颖2, 石先凤2, 沈虹2, 蔡兰兰2, 魏秀岩1
作者信息
  • 1.沈阳药科大学 生命科学与生物制药学院,辽宁 沈阳 110000
  • 2.北京阳光德美医药科技有限公司,北京 100071
通讯作者:
魏秀岩,副教授,硕士生导师 MP: 13194225280 E-mail:
作者简介:

陈学义(1992-),男,本科,初级药师,主要从事临床药代动力学生物样品分析方面的研究和工作

Determination of salmon calcitonin concentration in human plasma by HPLC-MS/MS method
Xue-yi CHEN1, 2, Xiao-xia JU2, Ying WANG2, Xian-feng SHI2, Hong SHEN2, Lan-lan CAI2, Xiu-yan WEI1
Affiliations
  • 1.College of Life Sciences and Biopharmaceuticals, Shenyang Pharmaceutical University, Shenyang 110000, Liaoning Province, China
  • 2.Beijing Scinovo Pharmaceutical Technology Co., Ltd., Beijing 100071, China
出版时间: 2026-06-17 doi: 10.13699/j.cnki.1001-6821.2026.11.013
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目的

建立测定鲑降钙素血药浓度的高效液相色谱串联质谱(HPLC-MS/MS)方法。

方法

用有机试剂沉淀血浆样品,离心分离取上清,再进行浓缩、复溶、进样,用phenomenex Jupiter® C4-300A色谱柱(2.1 mm×50.0 mm,5.0 μm)进行色谱分离,流动相为0.1%甲酸水(A)-0.1%甲酸乙腈(B);梯度洗脱,流速为0. 50 mL·min-1,柱温为50 ℃,进样量为20 μL。以定制的同位素化合物为内标,用电喷雾电离源,用正电离模式,以多反应监测的方式进行扫描。考察该方法的专属性、标准曲线、定量下限、精密度、准确度、回收率、基质效应和稳定性。

结果

方法的专属性结果良好,待测物与内标之间相互无干扰,鲑降钙素的标准曲线线性范围为2.00、4.00、10.00、50.00、100.00、200.00、360.00、400.00 pg·mL-1,标准曲线为y=2.98×10-2x+5.30×10-3R2=0.997 4),定量下限为2.00 pg·mL-1。日内、日间相对标准偏差(RSD)均小于15%,提取回收率为60.13%~75.39%(RSD<15%),基质效应为97.45%~109.72%(RSD<10%)。基质样品在实验台室温放置24 h、在-20 ℃和-70 ℃下反复冻融进行5次、在-20 ℃和-70 ℃冻存49 d以及处理后样品在自动进样器中放置333 h的稳定性经验证,准确度在97.03%~108.64%,均稳定。

结论

本研究建立的HPLC-MS/MS方法简单、快速、灵敏度高、专属性好,可用于药代动力学研究中血浆样本的检测。

鲑降钙素  /  高效液相色谱串联质谱法  /  血药浓度
Objective

To establish a high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of calcitonin salmon in human plasma.

Method

Precipitate plasma samples using organic reagents, then centrifuge and collect the supernatant, proceed with concentration, reconstitution, and sample injection, and a phenomenex Jupiter® C4-300A column (2.1 mm×50.0 mm, 5.0 μm) was used for chromatographic separation. The mobile phase was 0.1% formic acid water (phase A) -0.1% formic acid acetonitrile (phase B); gradient elution with a flow rate of 0.50 mL·min-1, column temperature 50 ℃, injection volume 20 μL. A custom-labeled isotopic compound was used as the internal standard, scanning was carried out by means of multi reaction monitoring (MRM) in the positive ionization mode with an electric spray ionization source(ESI). Examine the specificity, standard curve, lower limit of quantification (LLOQ), precision, accuracy, recovery rate, matrix effect, and stability of the method.

Result

The method showed a good specificity results of the method, and there is no interference between the analyte and the internal standard. The linear range of the standard curves for the tested substances was 2.00、4.00、10.00、50.00、100.00、200.00、360.00、400.00 pg·mL-1, The standard curve was y=2.98×10-2x+5.30×10-3 (R2=0.997 4) and the lower limit of quantification(LLOQ) is 2.00 pg·mL-1. The intra-day and inter day relative standard deviation (RSD) were both less than 15%, extraction recovery rates ranging from 60.13% to 75.39% (RSD<15%), and matrix effects ranging from 97.45% to 109.72% (RSD<10%). The stability of the matrix samples was verified by placing them at room temperature for 24 hours, repeatedly freezing and thawing at -20 ℃ and -70 ℃ for 5 times, freezing at -20 ℃ and -70 ℃ for 49 days, and placing the processed samples in an automatic sampler for 333 hours, with accuracy ranging from 97.03% to 108.64%, all stable.

Conclusion

The established HPLC-MS/MS method is simple, rapid, highly sensitive, and specific, and can be used for the detection of plasma samples in pharmacokinetic studies.

calcitonin salmon  /  high performance liquid chromatography tandem mass spectrometry  /  plasma concentration
陈学义, 举晓霞, 王颖, 石先凤, 沈虹, 蔡兰兰, 魏秀岩. 用HPLC-MS/MS法测定人血浆中鲑降钙素的浓度. 中国临床药理学杂志, 2026 , 42 (11) : 1581 -1585 . DOI: 10.13699/j.cnki.1001-6821.2026.11.013
Xue-yi CHEN, Xiao-xia JU, Ying WANG, Xian-feng SHI, Hong SHEN, Lan-lan CAI, Xiu-yan WEI. Determination of salmon calcitonin concentration in human plasma by HPLC-MS/MS method[J]. Chinese Journal of Clinical Pharmacology, 2026 , 42 (11) : 1581 -1585 . DOI: 10.13699/j.cnki.1001-6821.2026.11.013

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doi: 10.13699/j.cnki.1001-6821.2026.11.013
  • 接收时间:2026-03-26
  • 首发时间:2026-08-06
  • 出版时间:2026-06-17
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  • 收稿日期:2026-03-26
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    1.沈阳药科大学 生命科学与生物制药学院,辽宁 沈阳 110000
    2.北京阳光德美医药科技有限公司,北京 100071

通讯作者:

魏秀岩,副教授,硕士生导师 MP: 13194225280 E-mail:
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Number of
species
占总种数比例
Percentage of
total species (%)

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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