超高效液相色谱法快速测定抗痛风类中成药中16种非法添加化学药物  

Rapid determination of 16 chemical drugs in anti-gout in Chinese patent medicine by ultra performance liquid chromatography

作　　者：李文锐 罗廷顺 LI Wenrui;LUO Tingshun(Dali Institute for Drug Control,Dali 671000,China)

机构地区：[1]大理白族自治州药品检验所,云南大理671000

出　　处：《化学分析计量》2025年第2期41-46,共6页Chemical Analysis And Meterage

基　　金：云南省药品评价抽检计划项目(云药监办[2023]9号)。

摘　　要：建立超高效液相色谱法快速测定抗痛风类中成药中16种非法添加化学药物。通过甲醇超声提取样品,采用Agilent Eclipse XDB-C_(18)(150 mm×2.1 mm,1.8μm)色谱柱,以p H值为3.0的磷酸水溶液为流动相A,甲醇和乙腈的混合溶液(体积比1∶1)为流动相B,流量为0.25 m L/min,梯度洗脱,柱温为35℃,检测波长为220 nm,进样体积为1μL,二极管阵列检测器检测。16种化学药物的质量浓度在各自的线性范围内与对应的色谱峰面积呈现良好的线性关系,相关系数均大于0.999,检出限为0.01~0.18μg/m L,定量限为0.03~0.54μg/m L。样品的平均加标回收率为91.1%~99.3%,测定结果的相对标准偏差为0.8%~2.4%(n=6)。该方法快速准确,灵敏可靠,适用于抗痛风类中成药中非法添加化学药物的日常检验。An ultra-high performance liquid chromatography method was established for the rapid determination of 16 illegally added chemical drugs in anti-gout Chinese patent medicines.The samples were ultrasonically extracted with methanol.The chromatographic separation was performed on an Agilent Eclipse XDB-C_(18) column(150 mm×2.1 mm,1.8μm).The mobile phase consisted of phosphoric acid aqueous solution(pH 3.0)as mobile phase A and a mixture of methanol and acetonitrile(volume ratio 1:1)as mobile phase B,the flow rate was 0.25 mL/min,gradient elution.The column temperature was 35°C,the detection wavelength was 220 nm,the injection volume was 1μL,and the diode array detector was used for detection.The mass concentration of 16 chemical drugs showed a good linear relationship with the corresponding chromatographic peak area in their respective linear ranges,and the correlation coefficients were all more than 0.999,the detection limit was 0.01-0.18μg/mL,and the quantitative limit was 0.03-0.54μg/mL.The average recoveries of spiked samples were in the range of 91.1%-99.3%,and the relative standard deviations of determination results were in the range of 0.8%-2.4%(n=6).The method is rapid,accurate,sensitive and reliable,which is suitable for the daily inspection of illegally added chemical drugs in anti-gout Chinese patent medicines.

关 键 词：超高效液相色谱 二极管阵列检测器 抗痛风药类中成药 非法添加 

分 类 号：O657.7[理学—分析化学]