UPLC-DAD法快速测定减肥类保健食品中违法添加的8种化学药物

Rapid inspection of 8 illegally adulterated chemical drugs in weight controlling health food by ultra-high performance liquid chromatography-photodiode array detector

超高效液相色谱-二极管阵列（UPLC—DAD）同时快速测定减肥类保健食品中违法添加的8种化学药物（盐酸麻黄碱、咖啡因、呋塞米、盐酸芬氟拉明、酚酞、盐酸西布曲明、N-单去甲基盐酸西布曲明、N，N-双去甲基盐酸西布曲明）。采用ZORBAXSB—C18（2．1mm×100mm，1．8μm）色谱柱，流动相A：甲醇，流动相B：20mmol／L乙酸铵-0．1％乙酸，梯度洗脱，流速为O．4mL／min。采集210、225、265nm色谱图合成后进行初筛和定量。并根据8种药物的光谱特征建立光谱库，用于对应化合物的确证。结果表明：8种药物在16．1min内可有效分离，在其对应的线性范围内线性关系良好，相关系数（r）均大于0．9995，平均回收率在84．9％～109．3％之间，相对标准偏差均小于5％，检测限1～12ng。该方法简便、快速、灵敏度高且重现性好，可作为检测减肥类保健食品中违法添加化学药物的快速测定方法。

A rapid inspection method for the illegally adulterated chemical drugs in weight controlling health food was established using the ultra performance liquid chromatography coupled with photodiode array detector （UPLC-DAD）. In this study, 8 possible added chemical drugs （ephedrine hydrochloride, caffeine, furosemide, fenfluramine hydrochloride, phenolphthalein, sibutramine hydrochloride, N-desmethyl sibutramine Hydrochloride, and N-didesmethyl sibutramine hydrochloride） were simultaneously separated within a ZORBAX SB-C18 column （2.1 mm×100mm,1.8μm）, and the mobile phase was mixed the ratios of methanol and 20 mmol/L ammonium acetate -0.1% acetic acid. The elution rate was set as 0.4 mL/min, meanwhile the wavelength at 210 nm, 225 nm and 265 nm were selected for quantitive and 3D spectrum scaning within 190-400 nm for qualitative. The results indicated that during this condition, the 8 chemical drugs could be effectively separated within 16.1 min. The calibration curves during the appropriate concentration ranges showed a good linearity represented with the high correlation coefficients. The average recoveries were from 84.9% to 109.3% while represented with the low relative standard deviations （RSDs） values. The detection limits of the 8 chemical drugs ranged from 1 ng to 12 ng. Finally, we conclude that with this method, such illegally added chemical drugs in weight controlling health foods could simple and rapid inspected with high sensitivity and good reproducibility.