中国临床药理学杂志

用UPLC-MS/MS法测定人脑脊液中康替唑胺浓度

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贠菊平 ^1a , 王梓贺 ^1a , 王文静 ^1b , 刘炜 ^1a

中国临床药理学杂志 | 研究方法 2025,41(1): 91-95

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中国临床药理学杂志 |研究方法 2025 , 41 (1) : 91 -95

用UPLC-MS/MS法测定人脑脊液中康替唑胺浓度

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贠菊平^1a, 王梓贺^1a, 王文静^1b, 刘炜^1a

作者信息

^1a.首都医科大学附属北京佑安医院，药学部，北京 100069

^1b.首都医科大学附属北京佑安医院，临检中心，北京 100069

通讯作者:

刘炜，主任药师，硕士生导师 Tel: （010）83997776 E-mail: liuwei8090@126.com

作者简介:

贠菊平（1985-），女，博士研究生，主管药师，主要从事临床药学及治疗药物监测方面的相关研究

Determination of contezolid in human cerebro spinal fluid by UPLC-MS /MS

Ju-ping YUN^1a, Zi-he WANG^1a, Wen-jing WANG^1b, Wei LIU^1a

Affiliations

^1a.Department of Pharmacy, Beijing You’an Hospital, Capital Medical University, Beijing 100069, China

^1b.Clinical Laboratory Center, Beijing You’an Hospital, Capital Medical University, Beijing 100069, China

出版时间: 2025-01-17 doi: 10.13699/j.cnki.1001-6821.2025.01.019

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摘要

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目的

建立超高效液相色谱-串联质谱（UPLC-MS/MS）法测定人脑脊液中康替唑胺浓度的方法。

方法

以利奈唑胺为内标（IS），乙腈为蛋白沉淀剂。用Waters ACQUITY UPLC^® BEH C₁₈（2.1 mm×50.0 mm，1.7 μm）色谱柱进行分离，流动相为0.1%甲酸水溶液-0.1%甲酸乙腈溶液，梯度洗脱方式，流速为0.4 mL·min^-1，柱温为40 ℃，自动进样器温度为10 ℃，分析时间为4 min。用电喷雾离子源，正离子模式，多反应监测扫描方式。康替唑胺监测分析离子对为m/z 409.15→269.14，利奈唑胺监测离子对为m/z 338.14→195.10。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、基质效应、残留效应、稀释效应及稳定性。

结果

脑脊液中内源性物质对待测物利奈唑胺及内标物利奈唑胺的测定均无干扰，方法专属性好。康替唑胺在20~5 000 ng·mL^-1内线性关系良好，标准曲线为y=8.97×10^-4x+1.95×10^-2（r=0.999 1），定量下限为20 ng·mL^-1。批内、批间精密度相对标准偏差（RSD）均<15%，提取回收率为90.96%~98.71%。质控脑脊液样本的平均内标归一化基质效应因子为94.39%~100.25%。稀释效应的RSD均<15%。康替唑胺脑脊液样本在室温及自动进样器内72 h、-20 ℃和-80 ℃储存90 d、反复冻融3次均稳定，RSD均<10%。

结论

本方法灵敏度高、快速、简便、准确，适用于人脑脊液中康替唑胺治疗浓度监测。

关键词

康替唑胺 / 脑脊液 / 超高效液相色谱-串联质谱法 / 治疗药物监测

Abstract

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Objective

To establish a method for determining the concentration of contezolid in human cerebro spinal fluid (CSF) using ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS).

Methods

Linezolid as the internal standard (IS) and acetonitrile as the protein precipitant. Waters ACQUITY UPLC^® BEH C₁₈ (2.1 mm×50.0 mm, 1.7 μm) chromatographic column was used for separation, with a mobile phase of 0.1% formic acid aqueous solution-0.1% formic acid acetonitrile solution, gradient elution method, flow rate was 0.4 mL·min^-1, column temperature was 40 ℃, automatic sampler temperature was 10 ℃, the analysis time was 4 minutes. Electrospray ion source, positive ion mode, and multi-reaction monitoring scanning mode were used. The monitoring and analysis ion pairs for contezolid were m/z 409.15→269.14, and the monitoring ion pairs for linezolid were m/z 338.14→195.10. The specificity, standard curve and lower limit of quantification (LLOQ), precision and recovery rate, matrix effect, residual effect, dilution effect and stability of the method were investigated.

Results

The endogenous substances in CSF do not interfere with the determination of the analyte contezolid and the internal standard linezolid, and the method has good specificity. Satisfactory linearity was observed within the concentration range of 20-5 000 ng·mL^-1 for contezolid in CSF, the calibration curve was y=8.97×10^-4x+1.95×10^-2 (r=0.999 1), and the LLOQ was 20 ng·mL^-1. Precision of the intra-batch and inter-batch relative standard deviation (RSD)<15%, and the extraction recovery were 90.96%-98.71%. The average normalized matrix effect factor of the quality control CSF sample were 94.39%-100.25%. The RSD of dilution effect<15%. The CSF samples of contezolid were stored at room temperature, in the automatic sampler for 72 hours, -20 ℃ and -80 ℃ for 90 days, and subjected to repeated freezing and thawing three times, were stable with all of which the RSD<10%.

Conclusion

This method is high sensitivity, rapid, simple and accurate, which is very suitable for the therapeutic drug monitoring of contezolid in human CSF.

Key words

contezolid / cerebrospinal fluid / ultra high performance liquid chromatography tandem mass spectrometry / therapeutic drug monitoring

引用本文

贠菊平, 王梓贺, 王文静, 刘炜. 用UPLC-MS/MS法测定人脑脊液中康替唑胺浓度. 中国临床药理学杂志, 2025 , 41 (1) : 91 -95 . DOI: 10.13699/j.cnki.1001-6821.2025.01.019

Ju-ping YUN, Zi-he WANG, Wen-jing WANG, Wei LIU. Determination of contezolid in human cerebro spinal fluid by UPLC-MS /MS[J]. Chinese Journal of Clinical Pharmacology, 2025 , 41 (1) : 91 -95 . DOI: 10.13699/j.cnki.1001-6821.2025.01.019

基金

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首都医科大学北京佑安医院研究型病房示范建设基金资助项目(2-1-1-2n-03-10-03)

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2025年第41卷第1期

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文章信息

doi: 10.13699/j.cnki.1001-6821.2025.01.019

接收时间：2024-07-10
首发时间：2026-08-04
出版时间：2025-01-17

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收稿日期：2024-07-10

基金

首都医科大学北京佑安医院研究型病房示范建设基金资助项目(2-1-1-2n-03-10-03)

作者信息

^1a.首都医科大学附属北京佑安医院，药学部，北京 100069

^1b.首都医科大学附属北京佑安医院，临检中心，北京 100069

通讯作者:

刘炜，主任药师，硕士生导师 Tel: （010）83997776 E-mail: liuwei8090@126.com

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https://castjournals.cast.org.cn/joweb/zglcylxzz/CN/10.13699/j.cnki.1001-6821.2025.01.019

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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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