食品科学 ›› 2020, Vol. 41 ›› Issue (8): 297-302.doi: 10.7506/spkx1002-6630-20190103-031

• 安全检测 • 上一篇    下一篇

表面增强拉曼光谱法定性定量检测保健食品中非法添加物西地那非

胡家勇,张嫚,皮江一,彭青枝,冯灏,周陶鸿   

  1. (1.湖北省食品质量安全监督检验研究院,湖北 武汉 430075;2.湖北省食品质量安全检测工程技术研究中心,湖北 武汉 430075;3.湖北本质检测认证有限公司,湖北 武汉 430000)
  • 出版日期:2020-04-25 发布日期:2020-04-20
  • 基金资助:
    湖北省食品质量安全监督检验研究院自主立项项目(ZZLX2018004)

Quantitative and Qualitative Determination of Illicit Sildenafil in Health Foods by Surface Enhanced Raman Spectroscopy

HU Jiayong, ZHANG Man, PI Jiangyi, PENG Qingzhi, FENG Hao, ZHOU Taohong   

  1. (1. Hubei Provincial Institute for Food Supervision and Test, Wuhan 430075, China; 2. Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, China;3. Hubei Benchmark Certification & Inspection Co. Ltd., Wuhan 430000, China)
  • Online:2020-04-25 Published:2020-04-20

摘要: 建立表面增强拉曼光谱法定性定量检测保健食品中非法添加药物西地那非。利用拉曼光谱的特异性进行西地那非定性检测;用三聚氰胺作为内标物进行西地那非定量检测,以西地那非特征峰1 234 cm-1与三聚氰胺特征峰707 cm-1的峰高比为纵坐标,西地那非质量浓度为横坐标进行线性回归拟合,结果表明西地那非质量浓度在0~50 mg/L范围呈现良好的线性关系,R2=0.996 9。定性检测限为0.05 mg/L,定量检测限为5 mg/L。其固体、液体样品加标回收率分别为85.6%~92.6%、98.7%~105.2%,相对标准偏差分别为4.14%、3.25%。采用本方法对实际样品进行检测,其结果与高效液相色谱-质谱法测量结果基本一致。本方法准确、灵敏、快速,可用于保健品中非法添加西地那非类药物的定性定量检测。

关键词: 表面增强拉曼光谱法, 西地那非, 三聚氰胺, 保健食品, 定性检测, 定量检测

Abstract: In this paper, a method was established for the qualitative and quantitative determination of illicit sildenafil in health foods by surface enhanced Raman spectroscopy. By taking advantage of the specificity of Raman spectrum, we qualitatively determined sildenafil. Melamine was used as an internal standard to quantify sildenafil. Linear regression fitting was carried out using the peak height ratio between sildenafil at 1 234 cm-1 and melamine at 707 cm-1 as the y axis and sildenafil concentration as the x axis. Results indicated that a good linear relationship was observed in the concentration range of 0–50 mg/L with a correlation coefficient of 0.996 9. The limit of detection (LOD) was 0.05 mg/L, and the limit of quantitation (LOQ) was 5 mg/L. The recoveries of spiked solid and liquid samples were 85.6%–92.6% and 98.7%–105.2%, separately with relative standard deviations (RSD) of 4.14% and 3.25%, separately. In addition, this method was used to detect actual samples, and the results were basically consistent with those obtained by high performance chromatography-mass spectrometry (HPLC-MS). This method is accurate, sensitive and rapid, and can be used for the qualitative and quantitative detection of illicit sildenafil in health foods.

Key words: surface enhanced Raman spectroscopy, sildenafil, melamine, health foods, qualitative detection, quantitative detection

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