抗疲劳类保健食品中12种化药成分的液相快速筛查

颜伟华; 宋剑锋; 程闯; 郑明; 王笑笑; 方一超

doi:10.13386/j.issn1002-0306.2015.21.053

抗疲劳类保健食品中12种化药成分的液相快速筛查

Rapid screening of 12 anti- fatigue agents in health care products by HPLC

摘要

摘要: 采用高效液相色谱-二极管阵列检测器（HPLC-DAD）法,建立保健食品中12种化药成分的液相快速筛查方法。色谱条件:Agilent ZOBAX SB-C18色谱柱（4.6 mm×250 mm,5μm）,以乙腈、磷酸三乙胺溶液（取7 m L三乙胺用水稀释至1000 m L,用磷酸调p H至2.8±0.05）为二元梯度洗脱流动相,流速1.0 m L/min,柱温18℃,检测为波长230 nm。结果表明,12种抗疲劳化药成分在相应的浓度范围内,峰面积和进样量有良好的线性关系（r≥0.999）。检出限在4.02⁹.17 ng之间,回收率在98.69%¹09.07%之间,RSD在0.20%².46%之间。应用本方法从38批样品中检出1批非法添加化药成分西地那非。本法简单快速准确,精密度好,适用于基层药检机构,可以用于抗疲劳类保健食品中12种化药非法添加的快速筛查。

Abstract: A high- performance liquid chromatography- diode array detection ( HPLC- DAD) method was established for detection the simultaneous determination of 12 kinds anti- fatigue agents, which were illegally added in health care products.The sample were separated on Agilent ZOBAX SB- C18column ( 4.6 mm × 250 mm, 5 μm) , gradient eluted with mixture of acetonitrile and phosphoric acid- triethylamine ( 7 m L triethylamine, dilute with water to1000 m L, with phosphoric acid to regulate p H to 2.8 ± 0.05) at a flow rate of 1.0 m L / min. The column temperature was 18 ℃ and the detection wavelength was set at 230 nm.Results showed that good linearity was obtained for 12 kinds anti- fatigue agents in 12 components in a wide range and correlation was greater than 0.999.The LOD was from 4.02 to 9.17 ng.The recovery rate was from 98.69% to 109.07% and RSD was from 0.20% to 2.46%.Using this method, 1 batch of illegally added chemicals were detected from 38 batches of samples.This method was simple and precise, it can provide a reliable way for detecting 12 Anti- fatigue agents in health care products.