减肥类保健食品中非法添加酚酞定性定量检测方法的研究

 目的建立减肥类保健食品中非法添加酚酞的液质联用鉴别法及高效液相色谱含量测定法。方法对减肥类保健食品中添加的酚酞以液相色谱分离,采用离子阱质谱进行定性鉴别,流动相为0.5%甲酸-乙腈(70∶30),离子化模式为ESI(+),阱内击碎电压为0.86V;然后采用反相液相色谱对酚酞进行定量,流动相为水-乙腈(70∶30),检测波长为230nm。结果该质谱条件下,酚酞产生M+H]⁺分子离子峰,二级质谱的特征碎片离子明显。液相色谱定量法的线性范围为1.09～218mg·L^-1,平均回收率为99.57%。结论液质联用法定性准确、可靠;液相色谱含量测定方法简单、快速、重复性好。

Identification of Phenolphthalein in Diet Food by LC-MS/MS and Quantification by HPLC

OBJECTIVE To establish an identification method by LC-MS/MS and a quantification method by HPLC for phenolphthalein added illegally into the diet food for reducing weight.METHODS Identification was based on MS/MS spectra and retention times. The mobile phase consisted of 0.5% formic acid solution and acetonitrile (70∶30) , ESI(+), and MS/MS Frag Ampl was 0.86 V.The mobile phase of HPLC consisted of water and acetonitrile (70∶30) and the detection wavelength was 230 nm.RESULTS Phenolphthalein showed characteristic MS and MS/MS spectra.In the HPLC method,the linearity was over the range of 1.09～218 mg·L^-1, average recovery was 99.57%.CONCLUSION The method of LC-MS/MS is accurate and fast;and the HPLC method is simple, rapid and producible.