Article(id=1291404731268723469, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1291404681641713991, articleNumber=null, orderNo=null, doi=10.13699/j.cnki.1001-6821.2025.07.020, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1730217600000, receivedDateStr=2024-10-30, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1785824481073, onlineDateStr=2026-08-04, pubDate=1744819200000, pubDateStr=2025-04-17, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1785824481073, onlineIssueDateStr=2026-08-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1785824481073, creator=13701087609, updateTime=1785824481073, updator=13701087609, issue=Issue{id=1291404681641713991, tenantId=1146029695717560320, journalId=1246415772164075586, year='2025', volume='41', issue='7', pageStart='901', pageEnd='1050', issueExtLink='null', onlineDate='null', pubDate='1744819200000', pubDateStr='2025-04-17', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1785824469242, creator='13701087609', updateTime=1785824469242, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=1008, endPage=1012, ext={EN=ArticleExt(id=1291404731662988046, articleId=1291404731268723469, tenantId=1146029695717560320, journalId=1246415772164075586, language=EN, title=Determination of crizotinib in non-small cell lung cancer patients plasma by liquid chromatography tandem mass spectrometry, columnId=1246531413395263850, journalTitle=Chinese Journal of Clinical Pharmacology, columnName=Research Method, runingTitle=null, highlight=null, articleAbstract=
Objective

To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of crizotinib in human plasma and apply this method to determine its concentration in patients with non-small cell lung cancer after administrating.

Methods

Osimertinib was employed as the internal standard. The plasma samples were performed through protein precipitation with acetonitrile and chromatographed on Agilent Eclipse XDB C18 (2.1 mm×100.0 mm, 3.5 μm), mobile phase was consisted of acetonitrile containing 0.1% formic acid - 10 mmol·L-1 ammonium acetate containing 0.1% formic acid, flow rate was 0.25 mL·min-1, the column temperature was 30 ℃. The whole analytical time was 3 min. The detection was performed by positive ion electrospray ionization in multiple reaction monitoring mode, the quantitative analysis ion pairs were m/z 450.1→259.2 and m/z 500.2→72.1. The specificity, standard curve and lower limit of quantitation, precision and recovery, stability, matrix effect and residual effect of the method were investigated. After full validation, the method was applied to the determination of crizotinib in human plasma.

Results

Good linearity was observed over the concentration range of 10.0-2 500.0 μg·L-1, the calibration curve was y=4.54×10-3x+3.22×10-2 (r=0.992 7). The accuracies were between 97.66%-105.55%. The relative standard deviation of inter-day and intra-day precision were less than 8.49%. The average recoveries and matrix effects were between 80.10%- 86.05% and 95.22%-110.66%.

Conclusion

The LC-MS/MS method is developed which meets the requirements of biological sample analysis and it can quickly, accurately monitor the concentration of crizotinib.

, authors=Qi SHEN, Li LI, Jing LIANG, Min-yu CHENG, authorsList=Qi SHEN, Li LI, Jing LIANG, Min-yu CHENG, authorCompany=null, correspAuthors=Li LI, 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=1291404734267650831, articleId=1291404731268723469, tenantId=1146029695717560320, journalId=1246415772164075586, language=CN, title=用高效液相色谱串联质谱法测定非小细胞肺癌患者血浆中克唑替尼浓度, columnId=1246531413600784769, journalTitle=中国临床药理学杂志, columnName=研究方法, runingTitle=null, highlight=null, articleAbstract=
目的

建立一种测定人血浆中克唑替尼浓度的液相色谱串联质谱(LC-MS/MS)法,并用于非小细胞肺癌患者服药后的药物浓度测定。

方法

以奥希替尼为内标,血浆样品经乙腈蛋白沉淀预处理,色谱柱为Agilent Eclipse XDB C18柱(2.1 mm×100.0 mm,3.5 μm),流动相为10 mmol·L-1醋酸铵溶液含0.1%甲酸-乙腈含0.1%甲酸,流速为0.25 mL·min-1,柱温为30 ℃,进样时间为3 min。正离子模式的电喷雾电离源,多反应监测模式,克唑替尼及内标的离子对分别为m/z 450.1→259.2和m/z 500.2→72.1。考察该方法的专属性、标准曲线与定量下限、精密度与回收率、稳定性、基质效应、残留效应。该方法经完整验证后,用于克唑替尼的血药浓度测定。

结果

克唑替尼在10.0~2 500.0 μg·L-1内,线性关系良好,其标准曲线为y=4.54×10-3x+3.22×10-2r=0.992 7);准确度97.66%~105.55%,日内和日间精密度相对标准偏差均小于8.49%;克唑替尼平均提取回收率是80.10%~86.05%,基质效应在95.22%~110.66%。

结论

本LC-MS/MS方法符合生物样本分析要求,可以快速、准确地测定克唑替尼药物浓度。

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沈琦(1988-),女,主管药师,主要从事治疗药物监测与药代动力学的相关研究

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李力,主任药师,硕士生导师 Tel: (0571)87377360 E-mail:
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用高效液相色谱串联质谱法测定非小细胞肺癌患者血浆中克唑替尼浓度
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沈琦 , 李力 , 梁静 , 程敏毓
中国临床药理学杂志 | 研究方法 2025,41(7): 1008-1012
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中国临床药理学杂志 |研究方法 2025 , 41 (7) : 1008 -1012
用高效液相色谱串联质谱法测定非小细胞肺癌患者血浆中克唑替尼浓度
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沈琦, 李力 , 梁静, 程敏毓
作者信息
  • 浙江医院 药学部,浙江 杭州 310013
通讯作者:
李力,主任药师,硕士生导师 Tel: (0571)87377360 E-mail:
作者简介:

沈琦(1988-),女,主管药师,主要从事治疗药物监测与药代动力学的相关研究

Determination of crizotinib in non-small cell lung cancer patients plasma by liquid chromatography tandem mass spectrometry
Qi SHEN, Li LI , Jing LIANG, Min-yu CHENG
Affiliations
  • Depatment of Pharmacy, Zhejiang Hospital, Hangzhou 310013, Zhejiang Province, China
出版时间: 2025-04-17 doi: 10.13699/j.cnki.1001-6821.2025.07.020
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目的

建立一种测定人血浆中克唑替尼浓度的液相色谱串联质谱(LC-MS/MS)法,并用于非小细胞肺癌患者服药后的药物浓度测定。

方法

以奥希替尼为内标,血浆样品经乙腈蛋白沉淀预处理,色谱柱为Agilent Eclipse XDB C18柱(2.1 mm×100.0 mm,3.5 μm),流动相为10 mmol·L-1醋酸铵溶液含0.1%甲酸-乙腈含0.1%甲酸,流速为0.25 mL·min-1,柱温为30 ℃,进样时间为3 min。正离子模式的电喷雾电离源,多反应监测模式,克唑替尼及内标的离子对分别为m/z 450.1→259.2和m/z 500.2→72.1。考察该方法的专属性、标准曲线与定量下限、精密度与回收率、稳定性、基质效应、残留效应。该方法经完整验证后,用于克唑替尼的血药浓度测定。

结果

克唑替尼在10.0~2 500.0 μg·L-1内,线性关系良好,其标准曲线为y=4.54×10-3x+3.22×10-2r=0.992 7);准确度97.66%~105.55%,日内和日间精密度相对标准偏差均小于8.49%;克唑替尼平均提取回收率是80.10%~86.05%,基质效应在95.22%~110.66%。

结论

本LC-MS/MS方法符合生物样本分析要求,可以快速、准确地测定克唑替尼药物浓度。

克唑替尼  /  液相色谱串联质谱法  /  非小细胞肺癌  /  血药浓度
Objective

To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of crizotinib in human plasma and apply this method to determine its concentration in patients with non-small cell lung cancer after administrating.

Methods

Osimertinib was employed as the internal standard. The plasma samples were performed through protein precipitation with acetonitrile and chromatographed on Agilent Eclipse XDB C18 (2.1 mm×100.0 mm, 3.5 μm), mobile phase was consisted of acetonitrile containing 0.1% formic acid - 10 mmol·L-1 ammonium acetate containing 0.1% formic acid, flow rate was 0.25 mL·min-1, the column temperature was 30 ℃. The whole analytical time was 3 min. The detection was performed by positive ion electrospray ionization in multiple reaction monitoring mode, the quantitative analysis ion pairs were m/z 450.1→259.2 and m/z 500.2→72.1. The specificity, standard curve and lower limit of quantitation, precision and recovery, stability, matrix effect and residual effect of the method were investigated. After full validation, the method was applied to the determination of crizotinib in human plasma.

Results

Good linearity was observed over the concentration range of 10.0-2 500.0 μg·L-1, the calibration curve was y=4.54×10-3x+3.22×10-2 (r=0.992 7). The accuracies were between 97.66%-105.55%. The relative standard deviation of inter-day and intra-day precision were less than 8.49%. The average recoveries and matrix effects were between 80.10%- 86.05% and 95.22%-110.66%.

Conclusion

The LC-MS/MS method is developed which meets the requirements of biological sample analysis and it can quickly, accurately monitor the concentration of crizotinib.

crizotinib  /  liquid chromatography-tandem mass spectrometry  /  non-small cell lung cancer  /  plasma concentration
沈琦, 李力, 梁静, 程敏毓. 用高效液相色谱串联质谱法测定非小细胞肺癌患者血浆中克唑替尼浓度. 中国临床药理学杂志, 2025 , 41 (7) : 1008 -1012 . DOI: 10.13699/j.cnki.1001-6821.2025.07.020
Qi SHEN, Li LI, Jing LIANG, Min-yu CHENG. Determination of crizotinib in non-small cell lung cancer patients plasma by liquid chromatography tandem mass spectrometry[J]. Chinese Journal of Clinical Pharmacology, 2025 , 41 (7) : 1008 -1012 . DOI: 10.13699/j.cnki.1001-6821.2025.07.020
  • 浙江省中医药科技计划基金资助项目(2023ZL213; 2025ZL005)
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2025年第41卷第7期
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doi: 10.13699/j.cnki.1001-6821.2025.07.020
  • 接收时间:2024-10-30
  • 首发时间:2026-08-04
  • 出版时间:2025-04-17
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  • 收稿日期:2024-10-30
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浙江省中医药科技计划基金资助项目(2023ZL213; 2025ZL005)
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    浙江医院 药学部,浙江 杭州 310013

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李力,主任药师,硕士生导师 Tel: (0571)87377360 E-mail:
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
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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