高效液相色谱法测定降血压类健康产品中的6种二氢吡啶类成分

HPLC Determination of 6 Dihydropyridine Chemicals in Healthy Products for Anti-Hypertension

采用高效液相色谱法同时测定降血压类健康产品中非法添加的6种二氢吡啶类化学成分。样品经甲醇超声提取,提取液用ACE C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,柱温35℃,流动相为0.2%(ψ)磷酸溶液-乙腈混合液,梯度洗脱,流量1.0mL·min^(-1),采用二极管阵列检测器,检测波长为235 nm,以外标法定量。6种化合物的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)为56 mg·kg^(-1),测定下限(10S/N)为167 mg·kg^(-1)。加标回收率在96.0%~101%之间。测定值的相对标准偏差(n=6)在1.0%~1.2%之间。对阳性样品采用液相色谱-质谱法进行验证。

HPLC was applied to the simultaneous determination of 6 dihydropyridine chemicals, which were added illegally in healthy products for anti-hypertension. The 6 compounds in samples were extracted ultrasonically with methanol. The extracted solution was separated on an ACE C18 （250 mm）〈 4. 6 mm, 5 μm） chromatographic column with the column temperature of 35 ℃. A mixture of 0.2%（φ） phosphoric acid solution and acetonitrile was used as mobile phase for gradient elution with the flow rate of 1.0 mL ·min^-1. The 6 compounds were detected with DAD at the wavelength of 235 nm. Quantification analysis was performed by the external standard method. Linear relationships were found between the peak areas and the mass concentrations of the 6 compounds in definite ranges, with detection limits （3S/N） of 56 mg· kg^-1 and the low limits of determination （10S/N） of 167 mg · kg^-1. Recovery rates obtained by standard addition method were in the range of 96. 0%-101% and RSDs （n= 6） were in the range of 1.0 %-1.2%. The positive samples were further verified by LC-MS/MS.