碎米荠及富硒产品中无机硒提取方法的建立

采用不同浓度的HCl、NaOH、KH_2PO_4、NaHCO_3、KCl、流动相及超纯水作浸提液提取富硒产品中的无机硒后,用高效液相色谱-原子荧光光谱(HPLC-AFS)联用仪测定Se(IV)和Se(VI),并对浸提时间、浸提温度、振荡频率、液料比等条件进行系统研究,建立了富硒植物碎米荠及富硒产品中无机硒的提取方法:无机硒的最佳提取剂为0.1mol/L KH_2PO_4溶液,提取方法为:称取样品0.10g于离心管中,加入0.1mol/L KH_2PO_4溶液至3mL,于70℃、1 500r/min条件下振荡提取30min,以3 000r/min转速离心10min,0.45μm滤膜过滤后上机测定,样品加标回收率为86.14%~117.60%,Se(IV)和Se(VI)均能定性定量检测,为富硒产品中无机硒测定方法标准的制定奠定了基础。

Establishment of extraction methods of inorganic selenium in Cardamine and selenium-rich products

The Se(Ⅳ) and Se(Ⅵ) in selenium-rich health products and Cardamine were extracted by different concentrations of HC1,NaOH,KH2PO4,NaHCO3,KC1,liquid phase solution and pure water,etc,and determinated by high performance liquid chromatography-atomic fluorescence spectrometry(HPLC-AFS) united instrument.Extraction conditions such as time,temperature,and concentration were studied.The 0.1 mol/L KH2PO4 was the best extraction solution and the extraction method was as the following:adding 0.1 mol/L KH2 PO4 solution till 3 mL to 0.10 g sample in centrifuge tube,extracting 30 min at 1 500 r/min and 70 ℃ with oscillation,centrifuging for 10 min and determinating with HPLC-AFS after filtered through the 0.45 μm filter membrane.The recovery rate was between 86.14 ％ ～ 117.6 ％,and Se(Ⅳ)and Se(Ⅵ) can be qualitatively and quantitatively tested.