利用核-壳亚3微米填料色谱技术快速测定镇痛类健康产品中25种非法添加药物  

Rapid Determination of 25 Adulterated Drugs in Analgesic Health Products Based on Chromatography Technique with Fused-Core Sub-3 μm Filler

作　　者：温家欣[1] 陈林[2] 杨文杰[3] 雷毅 

机构地区：[1]广东省药品检验所,广州510180 [2]广东药学院药科学院,广州510006 [3]广州中医药大学,广州510006 [4]广东省食品检验所,广州510165

出　　处：《理化检验（化学分册）》2017年第6期621-626,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广东省省级科技计划项目(2013B090200059);广东省省级科技计划项目(2015A030401062);广州市健康产品非法添加化学成分快速检测技术重点实验室项目(2013年);广东省食品药品检验检测技术创新专项(2015ZX01)

摘　　要：采用核-壳亚3微米填料色谱柱建立了快速测定镇痛类健康产品中25种非法添加解热镇痛类药物及糖皮质激素类药物的高效液相色谱法。样品经甲醇超声提取,用Phenomenex Kinetex XB-C_(18)色谱柱(100mm×4.6mm,2.6μm)分离,流动相为乙腈-甲醇(2+1)溶液和0.2mol·L^(-1)乙酸铵溶液(pH 4.2),梯度洗脱。采用二极管阵列检测器,外标法定量。25种药物的线性范围为1.0~100mg·L^(-1),检出限(3S/N)为0.02~0.10g·kg^(-1)。加标回收率为90.6%~110%,测定值的相对标准偏差(n=6)为0.42%~2.5%。方法用于分析66批镇痛类健康产品,发现24批阳性样品,检出8种药物成分。High performance liquid chromatography （HPLC） method based on a fused-core sub-3 /am filler column was developed for the rapid determination of 25 drugs in analgesic health products. The samples were extracted ultrasonically with methanol, and the extract was separated on a Phenomenex Kinetex XB-Cls chromatographic column （100 mm× 4. 6 mm, 2. 6 μm） with acetonitrile/methanol （2＋ 1） and 0. 2 mol · L-1 ammonium acetate solution （pH 4. 2） as mobile phases for gradient elution~ Diode array detector was used. Quantification analysis was performed by the external standard method. The same linearity range of 25 drugs was 1.0-- 100 mg · L-1, with detection limits （3S/N） ranged from 0. 02 g · kg-1 to 0. 10 g · kg-1. Recovery rates obtained by standard addition method ranged from 90. 6% to 110% with RSDs （n=6） of 0. 42%--2. 5%. The method was applied for analysis of 66 analgesic health products, and 24 positive samples were found and 8 drugs were detected.

关 键 词：核-壳亚3微米填料 高效液相色谱法 解热镇痛类药物 糖皮质激素类药物 

分 类 号：O657.7[理学—分析化学]