中国临床药理学杂志

用HPLC-MS/MS法测定人血浆中尼可地尔浓度

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陈朝丽 ¹ , 王建欣 ¹ , 杨兰 ¹ , 张娜娜 ¹ , 史凌雪 ¹ , 段立广 ¹ , 安绯悦 ¹ , 伦杨 ¹ , 王佳琪 ¹ , 闫宇航 ¹ , 周春华 ¹^,²

中国临床药理学杂志 | 研究方法 2025,41(5): 712-716

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中国临床药理学杂志 |研究方法 2025 , 41 (5) : 712 -716

用HPLC-MS/MS法测定人血浆中尼可地尔浓度

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陈朝丽¹, 王建欣¹, 杨兰¹, 张娜娜¹, 史凌雪¹, 段立广¹, 安绯悦¹, 伦杨¹, 王佳琪¹, 闫宇航¹, 周春华¹^,²

作者信息

^1.河北医科大学第一医院临床药学部，河北石家庄 050000

^2.河北省人工智能临床药学技术创新中心，河北石家庄 050000

通讯作者:

周春华，主任药师 MP: 18633881377 E-mail: zhouchunhua@hebmu.edu.cn

作者简介:

陈朝丽（1997-），女，硕士研究生，药师，主要从事临床药学方面的研究

Concentration of nicorandil in human plasma was determined by HPLC-MS/MS

Chao-li CHEN¹, Jian-xin WANG¹, Lan YANG¹, Na-na ZHANG¹, Ling-xue SHI¹, Li-guang DUAN¹, Fei-yue AN¹, Yang LUN¹, Jia-qi WANG¹, Yu-hang YAN¹, Chun-hua ZHOU¹^,²

Affiliations

^1.Department of Clinical Pharmacy, The First Hospital of Hebei Medical University, Shijiazhuang 050000, Hebei Province, China

^2.The Technology Innovation Center for Artificial Intelligence in Clinical Pharmacy of Hebei Province, Shijiazhuang 050000, Hebei Province, China

出版时间: 2025-03-17 doi: 10.13699/j.cnki.1001-6821.2025.05.022

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摘要

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目的

建立测定人血浆中尼可地尔浓度的高效液相色谱-质谱（HPLC-MS/MS）法，并用于健康受试者的药代动力学研究。

方法

人血浆样品经乙腈萃取预处理。色谱柱：Acquity HPLC BEH C₁₈（1.7 μm，2.1 mm×50.0 mm），流动相：甲醇（含0.1%甲酸）-5 mmoL·L^-1乙酸铵（含0.1%甲酸）。流速：0.2 mL·min^-1，柱温：40 ℃，进样量：5 μL。梯度洗脱，电喷雾离子源，多反应监测，正离子扫描，内标为尼可地尔-d4同位素。考察该方法的专属性、标准曲线与定量下限、残留效应和稀释可靠性、精密度与回收率、基质效应、稳定性。

结果

建立的方法专属性好，尼可地尔在0.2~200.0 ng·mL^-1线性关系良好，其标准曲线为y=1.08×10^-1x＋2.66×10^-2（r=0.999 7），定量下限为0.2 ng·mL^-1，无残留效应，稀释后结果可靠，质控样品批内和批间精密度分别为0.64%~8.70%和0.91%~8.70%，批内和批间的准确度分别在100.00%~115.00%和98.00%~115.00%。尼可地尔在低、中、高质控浓度下的提取回收率为92.78%~95.35%，无明显基质效应，稳定性良好。

结论

该方法专属性高、准确度好、稳定、可重复、操作简单，可用于测定尼可地尔血浆中药物浓度。

关键词

尼可地尔 / 高效液相色谱-质谱法 / 血药浓度 / 药代动力学

Abstract

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Objective

To establish a high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method for the determination of nicorandil concentrations in human plasma and for pharmacokinetic studies in healthy subjects.

Methods

Human plasma samples were pretreated with acetonitrile extraction. Chromatographic cdumn: Acquity HPLC BEH C₁₈ (1.7 μm, 2.1 mm×50.0 mm), mobile phase: methanol (0.1% formic acid)-5 mmoL· L^-1 ammonium acetate (with 0.1% formic acid). Flow rate: 0.2 mL·min^-1, column temperature: 40 ℃, injection volume: 5 μL. Gradient elution, electrospray ion source, multiple reaction monitoring, positive ion scanning, nicorandil-d4 isotope as internal standard. The specificity of the method, the standard curve and the lower limit of quantification, the carryover effect and dilution reliability, the precision and recovery, the matrix effect, and the stability of the method were investigated.

Results

The specificity of the established method was good, nicorandil had a good linear relationship between 0.2-200.0 ng·mL^-1, the standard curve was y=1.08×10^-1x+2.66×10^-2 (r=0.999 7), the lower limit of quantification was 0.2 ng·mL^-1, there was no residual effect, the dilution results were reliable, and the intra-day and inter-day precision of quality control samples were 0.64%-8.70% and 0.91%-8.70%, respectively. The intra-day and inter-day accuracy were 100.00%-115.00% and 98.00%-115.00%, respectively. The extraction recoveries of nicorandil at low, medium and high quality control concentrations were 92.78%-95.35%, with no obvious matrix effect and good stability.

Conclusion

This method is highly specific, accurate, stable, reproducible, and simple to operate, and can be used to determine the concentration of drug in plasma of nicorandil.

Key words

nicorandil / high performance liquid chromatography-mass spectrometry / blood concentration / pharmacokinetics

引用本文

陈朝丽, 王建欣, 杨兰, 张娜娜, 史凌雪, 段立广, 安绯悦, 伦杨, 王佳琪, 闫宇航, 周春华. 用HPLC-MS/MS法测定人血浆中尼可地尔浓度. 中国临床药理学杂志, 2025 , 41 (5) : 712 -716 . DOI: 10.13699/j.cnki.1001-6821.2025.05.022

Chao-li CHEN, Jian-xin WANG, Lan YANG, Na-na ZHANG, Ling-xue SHI, Li-guang DUAN, Fei-yue AN, Yang LUN, Jia-qi WANG, Yu-hang YAN, Chun-hua ZHOU. Concentration of nicorandil in human plasma was determined by HPLC-MS/MS[J]. Chinese Journal of Clinical Pharmacology, 2025 , 41 (5) : 712 -716 . DOI: 10.13699/j.cnki.1001-6821.2025.05.022

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2025年第41卷第5期

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文章信息

doi: 10.13699/j.cnki.1001-6821.2025.05.022

接收时间：2024-09-27
首发时间：2026-08-04
出版时间：2025-03-17

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收稿日期：2024-09-27

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作者信息

^1.河北医科大学第一医院临床药学部，河北石家庄 050000

^2.河北省人工智能临床药学技术创新中心，河北石家庄 050000

通讯作者:

周春华，主任药师 MP: 18633881377 E-mail: zhouchunhua@hebmu.edu.cn

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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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