超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查保健品中136种非法添加降血压药物

Rapid screening of 136 kinds of illegally added antihypertensive drugs in health food by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

中文关键词:  超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法  快速筛查  降血压药物  非法添加

英文关键词:ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry  rapid screening  antihypertensive drugs  illegal addition

中文摘要:

      目的 建立一种无需标准品即可快速检测保健品中136种非法添加降血压药物的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱分析方法。方法 样品经甲醇溶液适当稀释, 超声处理后, 经Waters Acquity BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 以0.1% (V:V)甲酸水溶液-乙腈作为流动相, 进行梯度洗脱。将采集的样品质谱信息与自建立的136种非法添加降血压药物质谱信息库通过分子离子精准质量数比对、同位素分布比对进行初筛, 初筛出的阳性化合物通过二级碎片离子解析进行进一步确证。结果 该方法能够在没有标准品的情况下, 在20 min内对保健食品中136种非法添加降压药物同时进行精准筛查, 14种降压药物的添加回收实验表明实际样品的检出限在2.0~3.0 ?g/kg, 采用本方法对市售实际样品进行检验, 1款声称具有降血脂的保健食品中有坎地沙坦酯检出。结论 该方法通量高、速度快、成本低, 可用于保健食品中非法添加降血压药物的快速筛查。

英文摘要:

      Objective To establish a method for rapid determination of 136 kinds of illegally added antihypertensive drugs in health food without standards by ultra performance liquid chromatography-quadrupole/ electrostatic field orbitrap high resolution mass spectrometry. Methods Samples were diluted and extracted by ultrasound extraction with methanol solvent, separated on Waters Acquity BEH C18 chromatographic column (100 mm × 2.1 mm, 1.7 μm). Gradient elution was carried out with 0.1% (V:V) formic acid aqueous solution and acetonitrile as mobile phase. The acquired sample information and the self-established mass spectrometry information database of 136 kinds of illegally added antihypertensive drugs were preliminarily screened through accurate mass comparison and isotope distribution comparison. The positive compounds initially screened were further confirmed by secondary fragment ion analysis. Results This method could accurately screen 136 kinds of illegally added antihypertensive drugs in health food within 20 minutes without standards. The addition and recovery experiments of 14 kinds of antihypertensive drugs showed that the limit of detection of actual samples was 2.0?3.0 ?g/kg. This method was used to test the actual samples on the market, and candesartan ester was detected in one health food claimed to have blood lipid reduction. Conclusion The method has high throughput, high speed and low cost, and can be used for rapid screening of illegal blood pressure lowering drugs in health food.