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作 者:赵琪 吴光颖 张静怡 张超 陈卫 ZHAO Qi;WU Guang-ying;ZHANG Jing-yi;ZHANG Chao;CHEN Wei(Suzhou Institute for Drug Control,Suzhou 215000,Jiangsu,China)
机构地区:[1]苏州市药品检验检测研究中心,江苏苏州215000
出 处:《粮食与油脂》2024年第7期138-141,158,共5页Cereals & Oils
摘 要:采用超高效液相色谱-二极管阵列检测器(UPLC-DAD)建立同时测定辅助降血压类保健食品中20种非法添加化学药物的方法。采用Luna UPLC C18色谱柱(2.1 mm×100 mm,1.6μm),以质量分数为0.2%的磷酸水溶液-乙腈为流动相进行梯度洗脱。流速为0.21 mL/min,柱温为35℃,DAD扫描,检测波长为220 nm,各剂型样品经甲醇提取,通过保留时间和紫外吸收光谱定性,峰面积外标法定量。结果表明:20种药物成分能完全分离,在4~80μg/mL内线性关系良好,回收率为92.3%~104.1%,相对标准偏差(RSD)为1.3%~2.9%。1批阳性样品检出奈比洛尔、乐卡地平、拉西地平,并通过UPLC-MS/MS得到确证。建立的方法操作简便,精密度、稳定性、重复性好,能够达到快速检测降压类保健食品中非法添加化学成分的目的。A method for simultaneous determination of 20 kinds of illegally added chemical drugs in health food for blood pressure lowering was established by UPLC-DAD.Luna UPLC C18 column(2.1 mm×100 mm,1.6μm)was used for gradient elution with 0.2%mass fraction phosphoric acid aqueous solution and acetonitrile as mobile phase.The flow rate was 0.21 mL/min,the column temperature was 35℃,the DAD was used to scan,and the detection wavelength was 220 nm.Samples of each dosage form were extracted with methanol,qualitatively determined by retention time and UV absorption spectroscopy,and quantitatively determined by peak area external standard method.The results showed that 20 drug components could be completely separated,and the linear relationship was good in the range of 4-80μg/mL.The recoveries were 92.3%-104.1%,and the relative standard deviation(RSD)was 1.3%-2.9%.Nebilolol,lecardipine and lacidipine were detected in 1 batch of positive samples,which could be confirmed by UPLC-MS/MS.The established method was easy to operate,with good precision,stability and repeatability,and could achieve the purpose of rapid detection of illegal chemical ingredients in blood pressure bowering health food.
关 键 词:超高效液相色谱-二极管阵列检测器 降血压 非法添加 保健食品
分 类 号:TS207.7[轻工技术与工程—食品科学]
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