高效液相色谱-串联飞行时间质谱法检测安神类保健食品中非法添加物

Study on detection of illegal additives in sedative health food by LC-Q-TOF/MS

建立了安神类保健食品中的5种非法添加物(青藤碱、罗通定、扎来普隆、文拉法辛、褪黑素)的高效液相色谱—串联飞行时间质谱LC-Q-TOF/MS)的检测方法。用甲醇超声提取试样中5种违法添加物,以20mmol/L乙酸铵+0.1%(体积分数)甲酸溶液/甲醇溶液进行梯度洗脱,选用飞行时间质谱仪,采用电喷雾电离方式(ESI+),通过多反应监测(MRM)定量。结果表明:5种非法添加物在10～1 000μg/L时线性关系良好,相关系数>0.99;且空白样品的平均回收率为92.8%～110.1%,精密度为0.9%～1.8%。采用建立的方法对6种市售保健食品(胶囊、茶、口服液)进行检测,结果表明其中一种胶囊中含有非法添加物青藤碱,含量为1.656mg/kg。该方法选择性强、灵敏度高、处理方法简单、测定速度快。

LC-Q-TOF/MS was used to detect five illegal additives(rotundine,sinomenine, venlafaxine, melatonin,zaleplon)in sedative health food.The five illegal additives were extracted by ultrasound with a mixture of methanol and ammonium acetate20 mmol/L.A gradient system of a mixture of 0.1%formic acid with multi-reaction monitoring(MRM)was employed for quantitative determination at the ion source for ESI source,and the positive ion detection conditions were employed.The time-of-flight mass spectrometer was chosen,and the detecting parameters were set up and optimized.Qualitative and quantitative analysis of 5 kinds of illegal additives were carried out.The results showed that the five illegal additives were in good linear relationship within the range of 10~1 000μg/L and the correlation coefficient was greater than 0.99.The average recovery of the blank sample was between 92.8%~110.1%,and the precision was 0.9%~1.8%.Six kinds of commercially sold Sedative health food samples(A,B,C,D,E,F)were extracted by methanol and analyzed by LC-Q-TOF/MS.The results showed that a kind of capsule sample D contained sinomenine which content was1.656 mg/kg.Therefore,the method had the advantages of strong selectivity,high sensitivity,quick detection.