摘要
目的:针对减肥类中药制剂及保健食品,建立了可能非法添加的酚酞、西布曲明、N-单去甲基西布曲明、N,N-双去甲基西布曲明等4种成分的超高效液相色谱-质谱/质谱联用的检测方法。方法:色谱柱为Phenomenex Luna C_(18)(2)100A(150 mm×2.00 mm,3μm);柱温为35℃;流动相为10 mmol/L乙酸铵(以乙酸调节p H值至4.0)及乙腈,梯度洗脱;流速为0.2 m L/min;以优化后的质谱参数采集信号。结果:各成分检出限浓度为0.1~0.2 ng/m L;定量限浓度为0.3~0.5 ng/m L;线性范围为各成分定量限~100 ng/m L;在线性范围内相关系数均在0.99以上;平均加样回收率为94.2%~101.5%。结论:本方法简便,快速,准确,灵敏度高,专属性好,能用于减肥类中药制剂及保健食品中非法添加的快速检测。
Objective ：To develop a UPLC-MS/MS method for determination of four components（phenolphthalein, sibutratmine, N-Monodesmethylsibutramine and N, N- Didesmethylsibutramine） illegally mixed into traditional Chinese medicines and healthy foods for antiobesity. Methods ： Phenomenex Luna C_（18）（ 2） 100 A column（ 150 mm × 2. 00 mm, 3 μm） was used at a column temperature of 35 ℃, serving 10 mmol/L ammonium acetate（p H 4.0）-acetonitrile as a mobile phase. Gradient elution was adopted at a flow rate of 0.2 m L/min. Signals were collected by optimized MS/MS method. Results ：The detection limit of this method was 0.1 ~ 0.2 ng/m L,while the quantitative detection limit was 0.3 ~ 0.5 g/m L, and the linear range was the quantitative detection limit^100 ng/m L. All the correlation coefficients within the linear range was more than 0.99, and the average spike recovery was 94.2% ~ 101.5%. Conclusion ：This method is simple, rapid, accurate, and of high sensitivity and high specificity, which may be used for the rapid determination of illegal additives in the traditional Chinese medicines and healthy foods for antiobesity.
出处
《中国执业药师》
CAS
2016年第6期18-23,共6页
China Licensed Pharmacist
