表面增强拉曼光谱法快速测定保健酒中西地那非
目的 建立金核银壳结构纳米颗粒(Au@Ag NPs)的表面增强拉曼光谱法(surface-enhanced Raman scattering, SERS)快速检测保健酒中非法添加物西地那非的分析方法。方法 制备3种纳米粒子Ag、Au、Au@Ag NPs为SERS基底, 比较3种基底的增强效果。样品前处理基于溶剂萃取法, 利用二氯甲烷对保健酒中的西地那非进行简单提取, 通过调节体系pH值, 得到最佳提取率和SERS增强效果。结果 Au@Ag NPs的SERS增强效应优于Au NPs和Ag NPs; 用0.1 mol/L氢氧化钾调节溶液pH值可有效提高二氯甲烷的提取效果, 再用0.1 mol/L稀盐酸溶解挥发后残留物, 使得西地那非在pH调节后更有利于吸附在Au@Ag NPs表面, 获得更强的SERS信号。西地那非的检出限为0.5 mg/L, 在0.5~10 mg/L浓度范围内线性关系较好, 相关系数(r2)为0.9472, 回收率为86.0%~95.8%之间, 相对标准偏差(relative standard deviation, RSD)为3.6%~5.9%。 结论 SERS技术灵敏度高、特异性强, 可用于快速检测保健酒中的西地那非, 为快速筛查大量样品提供新方法。
Objective To establish a method for rapid determination of sildenafil in health wine by surface-enhanced Raman scattering (SERS) coupled with Au-Agcore-shell nanoparticles (Au@Ag NPs). Methods Three kinds of nanoparticles Ag, Au and Au@Ag NPs were prepared as SERS substrates, and the enhancement effects of the 3 substrates were compared. Based on solvent extraction, sildenafil in health wine was simply extracted with dichloromethane. By adjusting the pH of the system, the optimal extraction rate and SERS enhancement effect were obtained. Results Au@Ag NPs had better SERS enhancement than Au NPs and Ag NPs. Adjusting the pH by 0.1 mol/L potassium hydroxide solution could effectively improve the extraction effect of dichloromethane, and the residue was dissolved in 0.1 mol/L dilute hydrochloric acid, which made sildenafil more favorable for adsorption on the surface of Au@Ag NPs after pH adjustment, and obtained stronger SERS signal. The limit of detection of sildenafil was 0.5 mg/L, and the linear relationship was good in the range of 0.5-10 mg/L. The correlation coefficient (r2) was 0.9472, and the recoveries were 86.0%-95.8%, with RSDs 3.6%-5.9%. Conclusion The SERS technology is highly sensitive and specific, which can be used to quickly detect sildenafil in health wines, which providing a new method for rapid screening of large numbers of samples.
标题：表面增强拉曼光谱法快速测定保健酒中西地那非
英文标题：Rapid determination of sildenafil in health wine by surface-enhanced Raman scattering
作者：
郑娟梅 广西-东盟食品药品安全检验检测中心;;赛默飞世尔科技中国有限公司;;广西纯正堂制药有限公司;广西纯正堂制药有限公司
余婉松 赛默飞世尔科技中国有限公司
覃文霞 广西-东盟食品药品安全检验检测中心
彭义 广西纯正堂制药有限公司;广西纯正堂制药有限公司
袁光蔚 广西-东盟食品药品安全检验检测中心
王海波 广西-东盟食品药品安全检验检测中心
中文关键词:保健酒,西地那非,表面增强拉曼光谱,快速检测,
英文关键词:health wine,sildenafil,surface-enhanced Raman scattering,rapid detection,
发表日期：2018-09-30
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