摘要:
建立同时测定减肥类保健食品中非法添加化学药物氟西汀、比沙可啶以及蒽醌类成分番泻苷A、番泻苷B、大黄素、大黄素甲醚、大黄酸、大黄酚、芦荟苷和芦荟大黄素的高效液相色谱-二极管阵列检测器（HPLC-DAD）方法。采用Diamonsil C18色谱柱（250 mm×4.6 mm,5μm）,以乙腈（A）-0.02 mol/L乙酸铵溶液（含0.4%乙酸）（B）为流动相,梯度洗脱（05 min,85%B;525 min,85%B35%B;2550 min,35%B;5055 min,35%B85%B）,测定波长为268 nm,流速1.0 m L/min,柱温25℃。对HPLC-DAD检出氟西汀和比沙可啶的样品进行电喷雾飞行时间质谱（ESI-Q-TOF/MS）一级扫描及二级碎片离子比对进行阳性确证。结果表明:10种待测物线性关系良好（r≥0.995）,平均回收率位于90.3%104.7%之间,RSD均小于5.0%。实际样品测定发现25种减肥类保健食品中有2种检出氟西汀,1种检出比沙可啶,另有1种样品同时检出芦荟苷和芦荟大黄素。本文建立的方法具有较高的选择性和灵敏度,方法分离效果好,耐用性较强,能够用于减肥类保健食品中这10种成分的定性、定量测定。
Abstract:
An analytical method using high performance liquid chromatography coupled with diode array detector( HPLC- DAD) was developed for determination of illegally added chemical drugs fluoxetine and bisacodyl,and rhubarb anthraquinones such as sennoside A,sennoside B,emodin,emodin monomethyl ether,rheinic acid,chrysophanol,barbaloin and aloe- emodin in weight- loss functional foods. The separation was performed on a Diamonsil C18column( 250 mm × 4.6 mm,5 μm) by gradient elution of acetonitril and 0.02 mol / L ammonium acetate solution( containing 0.4% acetic acid) at a flow rate of 1.0 m L / min: 0~5 min,85% B,5~25 min,85% B~35% B,25~50 min,35% B,50~55 min,35% B~85% B.The detection wavelength was 268 nm and the column temperature was25 ℃. The samples containing fluoxetine or bisacodyl were confirmed by two grade of fragmention comparison using electrospray ionization- quadrupole- time of flight mass spectrometer( ESI- Q- TOF/ MS). The correlation coefficient of standard curve for each component in linearity range was not less than 0.995,as well as the average recoveries were 90.3% ~ 104.7% with the relative standard deviations( RSDs) were not more than 5.0%. After determination of 25 weight- loss functional foods,the fluoxetine and bisacodyl were detected in 2 and 1 samples,respectively.The barbaloin and aloe- emodin were both detected in one of the 25 samples.The method is reliable,sensitive,accurate and reproducible.It can be used for the qualitative and quantitative determination of above 10 components in weight- loss functional foods.
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