Rapid Detection of 30 Kinds of Anti Fatigue and Sleep Improving Drugs in Health Food by High Performance Liquid Chromatography Triple Quadrupole Composite Ion Trap Mass Spectrometry
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摘要: 利用高效液相色谱-三重四极杆复合离子阱质谱（HPLC-QTRAP），建立了快速检测保健食品中的30种缓解疲劳和改善睡眠类违禁添加药物的方法。采用乙腈和10 mmol/L乙酸铵溶液为流动相以250 μL/min流速进行梯度洗脱，经Phenomenex Kinetex C18柱（50 mm×2.1 mm，2.6 μm）分离，通过定时多反应监测（Scheduled MRM）采集、正负离子同时扫描、信息依赖性获取（IDA）触发增强型子离子扫描（EPI）模式分析数据，并形成EPI数据库用于定性确证，外标法定量。结果表明：30种化合物在胶囊、片剂、颗粒剂三种基质中线性良好，决定系数R2均大于0.996，检出限（LOD）为0.01~0.72 μg/kg，精密度（RSD）均小于6%，加标回收率为84.5%~104.7%，混合标准品溶液在24 h内稳定性良好。本方法检测速度快、通量大、灵敏度高，适用于保健食品中30种缓解疲劳和改善睡眠类违禁添加药物含量的测定，为新形势下的保健食品监管提供有效的技术支持。
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关键词:
- 高效液相色谱-三重四极杆复合离子阱质谱 /
- 违禁添加 /
- 化学药品 /
- 保健食品
Abstract: Using high performance liquid chromatography triple quadrupole composite ion trap mass spectrometry(HPLC-QTRAP),a rapid detection method of 30 kinds of drugs for anti fatigue and sleep improving was established. Acetonitrile and 10 mmol/L ammonium acetate solution were used as mobile phase to elute in gradient at a flow rate of 250 μL/min,and then chemical separated by Phenomenex Kinetex C18 column(50 mm×2.1 mm,2.6 μm).Through scheduled multiple reaction monitoring(Scheduled MRM)acquisition,simultaneous scan of positive and negative ions,information dependent acquisition(IDA)triggered enhanced product ion scan(EPI)mode the data was analyzed,and an EPI database was formed for qualitative confirmation.The results showed that the linearity of 30 compounds in capsule,tablet and granule was good,the coefficient of determination R2 was more than 0.996,the detection limit(LOD)was 0.01~0.72 μg/kg,the precision(RSD)was less than 6%,the recovery of standard addition was 84.5%~104.7%,the mixed reference solution had good stability within 24 h. This method has the advantages of fast detection speed,large flux and high sensitivity. It is suitable for the determination of 30 kinds of illegal added drugs in the health food of relieving fatigue and improving sleep,and provides effective technical support for the health food supervision under the new situation. -
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