CAJ | 학술논문

目的:建立测定减肥保健食品中非法添加酚酞和西布曲明的高效液相色谱.串联质谱分析方法,并通过研究其质谱特征,推测其裂解途径.方法:减肥咖啡、减肥茶、减肥胶囊、苹果醋咀嚼片、减肥蛋白素等不同类型的减肥保健食品经超声波辅助提取15min,以Waters Atlantis T3柱(150mm×2.1mm,3 μm)分离后,进行HPLCMS/MS多反应监测模式下的定性及定量分析.结果:酚酞在2.5～500 μg/L的范同内呈良好的线性关系,相关系数为0.9992;西布曲明在0.15～500 μg/L的范围内呈良好的线性关系,相关系数为0.9996.在低、中、高3个添加水平范围内的甲均回收率为82.3%～103.6%;日内精密度均小于5%,日问精密度均小于8%.在检测的20种样品中,检出含有西布曲明的样品13个,检出率为65%;含有酚酞的样品9个,检出率为45%.结论:本方法分析速度快、灵敏度高、回收率好,可用于不同减肥保健食品中非法添加酚酞和西布曲明的同时检测.
목적:건립측정감비보건식품중비법첨가분태화서포곡명적고효액상색보.천련질보분석방법,병통과연구기질보특정,추측기렬해도경.방법:감비가배、감비다、감비효낭、평과작저작편、감비단백소등불동류형적감비보건식품경초성파보조제취15min,이Waters Atlantis T3주(150mm×2.1mm,3 μm)분리후,진행HPLCMS/MS다반응감측모식하적정성급정량분석.결과:분태재2.5～500 μg/L적범동내정량호적선성관계,상관계수위0.9992;서포곡명재0.15～500 μg/L적범위내정량호적선성관계,상관계수위0.9996.재저、중、고3개첨가수평범위내적갑균회수솔위82.3%～103.6%;일내정밀도균소우5%,일문정밀도균소우8%.재검측적20충양품중,검출함유서포곡명적양품13개,검출솔위65%;함유분태적양품9개,검출솔위45%.결론:본방법분석속도쾌、령민도고、회수솔호,가용우불동감비보건식품중비법첨가분태화서포곡명적동시검측.
A simple and rapid method using high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was developed for the simultaneous determination of phenolphthalein and sibutramine illegally added to weigh loss functional foods.Along with this,mass spectral fragmentation pathways of the above analytes were elucidated.In the method,various samples,including weight loss coffee,tea,capsule and albumin as well as apple vinegar chewing tablets were extracted for 15 minutes using methanol with the assistance of ultrasonic.Qualitative and quantitative analysis was carded out for 20 samples in the MRM mode following chromatographic separation on a Waters Atlantis T3(150 mm×2.1mm,3μm)column.Linear ranges for phenolphthalein and sibutramine detected by the method were 2.5-500 μg/L and 0.15-500 μg/L,and corresponding correlation coefficients 0.9992 and 0.9996,respectively.Mean recoveries for both analytes in aforementioned 5 types of weight loss functional foods at three spike levels(low,medium and high)were within the range of 82.3%-103.6%(n = 6),with intraday precision RSDs less than 5% and inter-day precision RSDs less than 8%.Sibutramine was detected in 13 of 20 samples,and namely the detection ratio was 65%.Phenolphthalein was detected in 9 of 20 samples and namely the detection ratio was 45%.This method is characterized by rapidity,high sensitivity and recovery,and good reliability,thereby providing a robust approach for the determination of phenolphthalein and sibutramine illegally added to weight loss functional foods.