超高效液相色谱-二极管阵列检测器法快速测定保健食品中违法添加的14种性功能药物  

Rapid Determination of 14 Illegally Added Aphrodisiac Drugs in Functional Foods by Ultra-High Performance Liquid Chromatography-Photodiode Array Detector

作　　者：林芳 李涛 耿庆光 刘海静 朱小红 王松 

机构地区：[1]陕西省食品药品检验所,陕西西安710061

出　　处：《食品科学》2014年第4期163-169,共7页Food Science

基　　金：2014年陕西省科技统筹创新工程计划项目"陕西省食品药品快速检测公共服务平台建设"项目;陕西省社会科学基金项目(13G020)

摘　　要：建立超高效液相色谱-二极管阵列检测器检测方法同时、快速测定抗疲劳类及增强免疫力类保健食品中违法添加的14种性功能类化学药物（那红地那非、红地那非、伐地那非、羟基豪莫西地那非、枸橼酸西地那非、豪莫西地那非、氨基他达拉非、他达拉非、硫代艾地那非、伪伐地那非、那莫西地那非、康力龙、丙酸睾酮、苯丙酸诺龙）。采用ZORBAXSB-C18色谱柱，流动相A：乙腈-甲醇（90：10，V/V），B：0．7％三乙胺溶液（pH2．8），梯度洗脱，流速0．35mL／min。采集230nm波长处的色谱图进行初筛和定量。根据14种药物的光谱特征建立光谱库，确证检出化合物。结果表明：14种性功能药物在15．0min内可有效分离，在8～80μg／mL的线性范围内相关系数均大于0．9995，平均回收率为90．1％～106．5％，相对标准偏差为0．7％-4．9％，检测限为2～3ng。该方法简便、快速、灵敏度高且重复性好，可作为检测抗疲劳类及增强免疫力类保健食品中违法添加化学药物的快速测定方法。An ultra performance liquid chromatography-photodiode array detection method （UPLC-DAD） has been established for rapid and simultaneous determination of 14 illegally added aphrodisiacs （nor-acetylsildenafil, acetildenafil, vardenafil, hydroxyhomosildenafil, sildenafil citrate, homosildenafil, amino tadalafil, tadalafil, thioaildenafil, pseudovardenafil, norneosildenafil, stanozolol, testosterone propionate, and nandrolone phenylpropionate） in anti-fatigue and immunity promoting functional foods. ZORBAX SB-C18 column was applied with mobile phase A consisting of acetonitrile- methanol （90：10, V/V） and phase B consisting of 0.7% triethylamine （pH 2.8）. Linear gradient elution was used with a flow rate of 0.35 mL/min and detection wavelength of 230 nm for rapid screening and quantification of these drugs. Characteristic absorption spectral library of 14 aphrodisiac drugs have been established for identifying them. The results showed that the 14 aphrodisiac drugs could be effectively separated within 15.0 min, and the standard curves had good linearity over the concentration range of 8-80μg/mL. The correlation coefficients were all above 0.999 5. The average recoveries ranged from 90.1% to 106.5% with relative stand deviations （RSDs） of 0.7%-4.9%. The detection limits for the 14 aphrodisiacs drugs ranged from 2 to 3 ng. These results indicate that the method is simple and rapid with high sensitivity and good reproducibility, and suitable for the rapid and simultaneous determination of the 14 illegally added aphrodisiac drugs in anti- fatigue and immunity-improving health foods.

关 键 词：保健食品 性功能药物 违法添加 快速测定 超高效液相色谱-二极管阵列检测器 

分 类 号：TS207.7[轻工技术与工程—食品科学] O657.72[轻工技术与工程—食品科学与工程]