基于亚3 μm核壳填料色谱柱技术建立了高效液相色谱法快速筛查21种抗风湿类化合物.供试品以1%乙酸-甲醇为提取溶剂,经ACCHROM C18 100A (4.6 mm×100 mm,2.8 μm)分离,以磷酸水溶液(pH 3.0)-甲醇-乙腈溶液为流动相,梯度洗脱,检测波长为230 nm,流速1.0 mL/min,柱温35 ℃.该方法在20 min内可分离21种成分,各化合物的线性范围为5~100 μg/mL(萘普生为1.5~30 μg/mL),回收率为91.0%~109.1%.萘普生的检出限(S/N=3)为0.8 mg/kg,其余化合物的检出限为2.0 mg/kg.按上述方法对抽检样品进行检测,发现18批阳性样品,并采用液相色谱-质谱联用法进一步确证.该方法快速、准确,适用于抗风湿类中成药或保健食品中非法添加化学成分的快速筛查,具有广阔的应用前景.%A method for the rapid determination of 21 adulterants in anti-rheumatic Chinese patent drugs or dietary supplements was established by HPLC using sub-3 μm fused-core silica particles columns.The samples were extracted with 1% acetic acid-methanol,and separated on the fused-core column ACCHROM C18 100A (4.6 mm×100 mm,particle size 2.8 μm) column by gradient elution with a water solution of phosphoric acid (pH 3.0)-methanol-acetonitrile as mobile phase at a flow rate of 1.0 mL/min.The detection wavelengths were set at 230 nm and the column temperature was set at 35 ℃.Under the conditions,21 compounds could be separated within 20 min,and the calibration curve of naproxen showed a good linearity in the range of 1.5-30 μg/mL while those of the other 20 compounds were in the range of 5-100 μg/mL,and the detection limits(S/N=3) were 0.8 mg/kg for naproxen and 2.0 mg/kg for other compounds.The recoveries were between 91.0% and 109.1%.The method was applied in the detection of real samples,and 18 positive samples were found.The samples were further confirmed by HPLC-MS/MS.The results indicated that this method was rapid and accurate,and could be used for the rapid determination of illegal adulteration in anti-rheumatic Chinese patent drugs or dietary supplements,which indicates its extensive application prospect.
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