| 孙莉,张蓉,胡杰,等.超高效液相色谱 -串联质谱法在检测保健食品和中成药中非法添加降压药研究[J].安徽医药,2026,30(1):73-77. |
| 超高效液相色谱 -串联质谱法在检测保健食品和中成药中非法添加降压药研究 |
| Detection of antihypertension chemicals in adulterated dietary supplement and Chinese patent medicines by UPLC-MS-MS |
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| DOI:10.3969/j.issn.1009-6469.2026.01.015 |
| 中文关键词: 抗高血压药 色谱法,高压液相 串联质谱法 保健食品 中成药 非法添加物 药物污染 |
| 英文关键词: Antihypertensive agents Chromatography, high pressure liquid Tandem mass spectrometry Health food Tradi-tional Chinese patent medicines and simple preparations Illegal ingredient Drug contamination |
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| 中文摘要: |
| 目的建立一种检测在保健食品和中成药中非法添加 15种降压药物的分析方法。方法研究时间为 2023年 1—11月,样品用甲醇超声提取,采用超高效液相色谱 -串联质谱( UPLC-MS-MS)法,以 Shim-pack XR-ODSⅢ(75 mm×2.0 mm,1.6 μm)为色谱柱, 0.3%甲酸水溶液 -乙腈为流动相,梯度洗脱;流速为 0.2 mL/min,柱温 40 ℃。选择电喷雾离子( ESI)源,采用正、负离子扫描,多反应监测( MRM)模式,测定 15种常用的降压药物。结果 15种药物在 17 min内达到理想的分离效果。方法线性范围宽,相关性好( r≥0.998);以 3个添加水平测定样品的回收率和相对标准差( RSD),回收率为 91.33%~113.07%,RSD均小于 5%。各药物检测限为 0.26~243.20 μg/L。结论该方法简便、专属性强、灵敏度高,可用于保健食品和中成药中非法添加降压药物的准确定性、定量检测。 |
| 英文摘要: |
| Objective To establish a rapid analysis method to determine 15 antihypertension chemicals in adulterated dietary supple-ment and Chinese patent Medicines.Methods The samples were extracted with methanol by ultrasound from January to November 2023. The ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method was adopted and the separation was fulfilled on a Shim-pack XR-ODSⅢ (1.6 μm 75 mm×2.0 mm) column with the mobile phase consisting of 0.3% formic acid watersolution (A) and acetonitrile (B). Gradient elution was used with the flow rate 0.2 mL/min, and the column temperature was set at 40 ℃.Results 15 antihypertension chemicals were well separated within 17 minutes. The linear range of mass spectrometry for 15 chemi-cals was wide, and the correlation was good (r≥0.998). The recovery rate and relative standard deviation of the samples were determinedby three addition levels, with the recovery rate ranging from 91.33% to 113.07% and the relative standard deviation (RSD) being lessthan 5%. The detection limits of each drug ranged from 0.26 to 243.20 μg/L.Conclusion The method is simple, rapid, specific andsensitive. It is suitable for the determination of 15 illegally added antihypertension chemicals in health foods and Chinese patent Medi-cines. |
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