液相色谱法测定保健食品中脱氢表雄酮含量

Determination of dehydroepiandrosterone content in health foods by liquid chromatography

中文关键词:  保健食品  脱氢表雄酮  液相色谱

英文关键词:health food  dehydroepiandrosterone  liquid chromatography

中文摘要:

      目的 建立液相色谱法检测多种类型保健食品中脱氢表雄酮(dehydroepiandrosterone, DHEA)含量的分析方法。方法 片剂和胶囊采用乙腈:水(60:40, V:V)提取; 口服液用乙腈提取, 加入氯化钠使乙腈水分层; 凝胶糖果用温水溶解后, 乙腈提取, 利用硫酸铵沉淀明胶且实现乙腈水分层, 最终有效提取保健食品中DHEA, 利用液相色谱二极管阵列检测或液相色谱-串联四极杆质谱法测定, 外标法定量。结果 建立的方法能有效提取检测保健食品中DHEA, 液相色谱二极管阵列检测固体或粉末样品方法检出限为0.15 g/kg, 定量限为0.5 g/kg; 液体样品方法检出限为1.5 mg/L, 定量限为5 mg/L; 方法回收率为95.7%~104.0%, 相对标准偏差为1.10%~3.76%。将该方法用于实际样品检测, 发现大多数电商平台的膳食补充剂中DHEA的含量与标签一致, 少量样品与标签不符。结论 该方法灵敏, 简单便捷, 不仅可用于监测国内功能性保健食品中DHEA的非法添加, 同时可实现对跨境膳食补充剂中DHEA的含量评价。

英文摘要:

      Objective To establish an analytical method for the determination of dehydroepiandrosterone (DHEA) content in variety of health food by liquid chromatography. Methods Tablets and capsules were extracted with acetonitrile:water (60:40, V:V); oral liquid was extracted with acetonitrile and added sodium chloride to salt out the targets from water; gel candy was dissolved in warm water first, and extracted with acetonitrile, after that ammonium sulfate was used to precipitate gelatin and made acetonitrile water stratification simultaneously. Finally, DHEA in health product was effectively extracted, then determined by liquid chromatography with diode array detection or liquid chromatography tandem mass spectrometry and quantified by external standard method. Results The established methods were effective in extracting DHEA from health foods, with limit of detection for solid or powder sample was 0.15 g/kg and for liquid was 1.5 mg/L and limit of quantification was 0.5 g/kg for solid or powder samples and 5 mg/L for liquid, respectively. The recovery of this method was 95.7%–104.0%, and the relative standard deviation was 1.10%–3.76%. It was found that the content of DHEA in imported dietary supplements was mostly consistent with the label, with a few samples not matching the label in real sample. Conclusion This method is sensitive, simple and convenient, and can be used not only to monitor the illegal addition of DHEA in domestic health foods, but also to evaluate the content of DHEA in cross-border dietary supplements.