| 血清胆汁酸谱系测定在肝硬化诊断中的应用价值 |
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| 引用本文： | 牟燕, 吴瑛瑕, 张易天, 曾颖炫, 周枝凤. 血浆中6种初级胆汁酸HPLC–MS/MS测定[J]. 中国公共卫生, 2023, 39(1): 102-106. DOI: 10.11847/zgggws1138567 |
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| 作者姓名： | 牟燕 吴瑛瑕 张易天 曾颖炫 周枝凤 |
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| 作者单位： | 1.南方医科大学 公共卫生学院 卫生检验检疫系，广东 广州 510515 |
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| 基金项目： | 国家自然科学基金（21607070） |
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| 摘 要： | 目的 建立高效液相色谱 – 串联质谱法快速检测血浆中6种初级胆汁酸的含量。 方法 血浆经甲醇沉淀蛋白后，用Thermo Accucore C18色谱柱（100 mm × 4.6 mm，2.6 μm）进行色谱分离，流动相为甲醇 – 水（0.1 %甲酸 + 5 mmol/L乙酸铵），梯度洗脱。负离子模式下多反应监测模式检测。实测6名健康成年人和6只成年SD大鼠样本。 结果 6种初级胆汁酸在6 min内实现基线分离，在5～2 000 μg/L范围内线性良好，相关系数＞0.995，检出限为0.25～0.45 μg/L，定量限为0.84～1.49 μg/L。日内、日间加标回收率分别为86.3 %～111.5 %和87.7 %～104.9 %；日内、日间相对标准偏差分别为5.2 %～11.9 %和6.6 %～14.3 %。健康成年人和成年SD大鼠血浆中初级胆汁酸的浓度显著不同。 结论 该方法简单、快速、灵敏、准确，可用于临床检验和动物试验中初级胆汁酸的快速检测。
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| 关 键 词： | 高效液相色谱-串联质谱法 初级胆汁酸 血浆 |
| 收稿时间： | 2022-03-20 |
The continuing importance of bile acids in liver and intestinal disease |
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| MU Yan, WU Ying-xia, ZHANG Yi-tian, ZENG Ying-xuan, ZHOU Zhi-feng. Simultaneous and rapid determination of 6 primary bile acids in plasma by high-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Public Health, 2023, 39(1): 102-106. DOI: 10.11847/zgggws1138567 |
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| Authors: | MU Yan WU Ying-xia ZHANG Yi-tian ZENG Ying-xuan ZHOU Zhi-feng |
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| Affiliation: | 1.Department of Hygiene Inspection and Quarantine Science, School of Public Health, Southern Medical University, Guangzhou, Guangdong Province 510515, China |
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| Abstract: | Objective To develop a rapid and accurate high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the simultaneous determination of 6 primary bile acids in plasma. Methods Plasma was separated on a Thermo Accucore C18 column (100 mm × 4.6 mm; 2.6 μm) after being extracted by protein precipitation using methanol. The 6 primary bile acids were separated by using the mobile phase of methanol-water (0.1% formic acid + 5 mmol/L ammonium acetate) running in gradient elution. The mass spectrometer was operated on an electrospray ionization source in negative ion mode for the multiple reaction monitoring analysis. Plasma from 6 healthy adults and 6 adult Sprague-Dawley (SD) rats was detected. Results Baseline separation of 6 primary bile acids was achieved within 6 min. The linearity of the calibration curves of the 6 primary bile acids was excellent in the range of 5 – 2000 μg/L with a correlation coefficient higher than 0.995. The limits of detection and limits of quantitation were in the range of 0.25 – 0.45 μg/L and 0.84 – 1.49 μg/L, respectively. The recoveries of intra-day and inter-day were 86.3% – 111.5% and 87.7% – 104.9%, with relative standard deviations of 5.2% – 11.9% and 6.6% – 14.3%, respectively. The concentrations of primary bile acids in plasma of healthy adults and adult SD rats were significantly different. Conclusion This method is simple, rapid, sensitive, and accurate, and can meet the needs for rapid detection of primary bile acids in clinical tests and animal experiments. |
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| Keywords: | HPLC-MS/MS primary bile acid plasma |
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