亚3_μm填料核壳色谱柱结合HPLC-DAD法快速测定降压类中成药及保健食品中添加的34种化学药物

目的：采用亚3 μm填料核壳色谱柱建立快速检测降压类中成药及保健食品中非法添加的34种化学药物的HPLC-DAD方法。方法：样品以甲醇为溶剂超声提取，采用Shiseido Capcell Core C₁₈色谱柱（150 mm×4.6 mm，2.7 μm）分离，以甲醇-0.02 mol·L^-1乙酸铵（用甲酸调节pH=3.0±0.1）为流动相梯度洗脱，流速0.7 mL·min^-1，柱温40℃，检测波长215、230 nm，二极管阵列扫描光谱进一步确证。结果：34种化学降压药在相应浓度范围内呈良好线性关系，相关系数均大于0.998，检测下限为0.1~10.5 ng·mL^-1，3个浓度水平回收率（n=6）在82.7%~118.9%之间，RSD为0.50%~4.1%。收集的94批样品中有16批呈非法添加阳性，其中卡维地洛为首次报道检出，5批阳性样品存在不同降压机制化学药的组合添加。结论：本方法可用于降压类中成药及保健食品中非法添加化学药的高通量筛查和定量检测。

Objective:To develop a method for rapid determination of 34 chemical drugs which were illegally added into anti-hypertensive Chinese patent medicines and health foods by HPLC-DAD coupled with sub-3 μm particle fused-core column. Methods:After ultrasonic extraction by methanol, the sample was separated on a Shiseido Capcell Core C₁₈ (150 mm×4.6 mm, 2.7 μm) column with gradient elution.The mobile phase consisted of methanol and 0.02 mol·L^-1 ammonium acetate solution (using formic acid to adjust pH=3.0±0.1) at a flow rate of 0.7 mL·min^-1. The column temperature was set at 40℃ and the wavelengths were set at 215 nm and 230 nm. The peaks were simultaneously confirmed by the spectrum range from diode array detection (DAD).Results:A good resolution of 34 chemical drugs was obtained. The correlation coefficients for 34 chemical drugs were above 0.998 in linearity range. And the limits of detection ranged from 0.1-10.5 ng·mL^-1. The recoveries were 82.7%-118.9%, with the relative standard deviations of 0.5%-4.1% at three spiked levels. Illegally adulteration of chemical drugs was found in 16 from 94 tested samples. Carvedilol was detected for the first time. Chemical drugs with different anti-hypotensive mechanisms were synergistically adulterated in 5 batches of positive samples. Conclusion:The method is suitable for confirmation of 34 illegally added chemical drugs in anti-hypertensive Chinese patent medicines and healthy foods.

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