安神类保健品中违禁化学药物的HPLC-DAD法测定研究

Determination of prohibited chemicals in sleep-improving health-food by HPLC-DAD

目的建立安神类保健品中违禁化学药物的HPLC-DAD测定方法。方法色谱柱为Thermo C_(18)(250 mm×4.6 mm,5μm),流动相A为乙腈,流动相B为含0.1%乙酸的0.01 mol·L^(-1)乙酸铵水溶液,梯度洗脱,流速1.0 mL·min^(-1),柱温35℃,检测器DAD,检测波长220 nm,进样量10μL。结果青藤碱、佐匹克隆、褪黑素、文法拉辛、氯苯那敏、罗通定、扎来普隆线性范围依次为1.42～57.0μg·mL^(-1)(R^2=0.9996)、1.52～60.7μg·m L^(-1)(R^2=0.9995)、1.41～56.4μg·mL^(-1)(R^2=0.9999)、1.36～54.3μg·mL^(-1)(R^2=0.9998)、1.52～60.9μg·m L^(-1)(R^2=0.9999)、1.75～70.0μg·mL^(-1)(R^2=0.9996)、1.58～63.0μg·mL^(-1)(R^2=1.0000),加样回收率均大于91.0%,RSD均小于1.8%。结论本方法灵敏度、准确度高、重复性好,为安神类保健品的质量控制提供了更为科学快捷的方法。

Objective To establish an HPLC-DAD method to determine the prohibited chemicals in sleepimproving health-food. Methods Thermo C_（18）（250 mm×4.6 mm, 5 μm） was used. Mobile phase A was acetonitrile; mobile phase B was 0.01 mol·L-（-1） ammonium acetate aqueous solution containing 0.1% acetic acid. Gradient elution was performed at a flow rate of 1.0 mL·min-（-1）. The column oven temperature was 35 ℃, DAD, the detection wavelength was 220 nm, and the injection volume 10 μL. Results Sinomenine, zopiclone, melatonin, venlafaxine, chlorpheniramine, lootidine, and zaleplon showed good linearity at 1.42-57.0 μg·mL^-1（R^2= 0.9996）, 1.52-60.7 μg·mL^-1（R^2= 0.9995）, 1.41-56.4 μg·mL^-1（R^2= 0.9999）, 1.36-54.3 μg·mL^-1（R^2= 0.9998）, 1.52-60.9 μg·mL^-1（R^2= 0.9999）, 1.75-70.0 μg·mL^-1（R^2= 0.9996）, and 1.58-63.0 μg·mL^-1（R^2= 1.0000）. The recoveries were more than 91.0%, and RSD less than 1.8%. Conclusion The method has good sensitivity, accuracy and reproducibility, which can control the quality of sleep-improving health-food.