食品科学

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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

林 芳,李 涛*,耿庆光,刘海静,朱小红,王 松   

  1. 陕西省食品药品检验所,陕西 西安 710061
  • 出版日期:2014-02-25 发布日期:2014-03-17
  • 通讯作者: 李 涛
  • 基金资助:

    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)

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

LIN Fang, LI Tao*, GENG Qing-guang, LIU Hai-jing, ZHU Xiao-hong, WANG Song   

  1. Shaanxi Institute for Food and Drug Control, Xi’an 710061, China
  • Online:2014-02-25 Published:2014-03-17
  • Contact: LI Tao

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ZORBAX SB-C18色谱柱,流动相A:乙腈-甲醇(90﹕10,V/V),B:0.7%三乙胺溶液(pH 2.8),梯度洗脱,流速0.35 mL/min。采集230 nm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15.0 min内可有效分离,在8~80 μg/mL的线性范围内相关系数均大于0.999 5,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2~3 ng。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。

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

Abstract:

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 acetonitrilemethanol
(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 8–80 μg/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 antifatigue
and immunity-improving health foods.

Key words: health food, aphrodisiacs drugs, illegally added, rapid determination, ultra performance liquid chromatographyphotodiode array detector (UPLC-DAD)

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