表面增强拉曼光谱快速检测抗风湿类中成药中非法添加的美洛昔康
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O 657.37

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Surface-Enhanced Raman Spectroscopy for Rapid Detection of Illegally Added Meloxicam in Anti-Rheumatic Chinese Patent Medicines
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    摘要:

    为了有效防范中成药以及保健品中非法添加美洛昔康,开发了一种灵敏、便捷、准确的美洛昔康的检测方法。通过金属辅助的化学刻蚀制备银纳米枝晶修饰的硅纳米阵列(AgNDs/SiNWs)作为表面增强拉曼光谱的增强基底,目标物美洛昔康作为拉曼探针分子,通过优化制备条件以及检测条件,评价其拉曼增强效果、重现性、可重复利用性以及储存稳定性。选择HF-H2O2-H2O体系作为刻蚀液,采用两步法,刻蚀时间25 min,镀银时间120 s的刻蚀条件,将5 μL美洛昔康滴加在AgNDs/SiNWs上进行拉曼检测,最低检测质量浓度为0.1 μg/mL,其中,1 160 cm-1处拉曼峰强度与美洛昔康质量浓度在0.1~25 μg/mL线性关系较好(y=8.688 7x+89.945 9,R2=0.992 3)。对市售抗风湿类中成药复方蚂蚁活络胶囊中的美洛昔康进行检测,样品未测出美洛昔康成分,即低于16.7 μg/g,远低于一般非法添加量7.5 mg/g。加标回收率为80.0%~112.4%,验证了该方法在实际样品检测中的可行性。

    Abstract:

    In order to effectively prevent the illegal addition of meloxicam in Chinese patent medicines and healthcare products, a sensitive, convenient and accurate method for detecting meloxicam was developed. Silver nanodendrite-modified silicon nanoarrays(AgNDs/SiNWs) were prepared by metal-assisted chemical etching and used as the enhanced substrate for surface-enhanced Raman spectroscopy. Meloxicam was utilized as the Raman probe molecule. The Raman enhanced effect, reproducibility, reusability and storage stability were evaluated by optimizing the preparation and detection conditions. The HF-H2O2-H2O system was chosen as the etching solution. A two-step method was adopted with etching time of 25 min and silver plating time of 120 s, and 5 μL of meloxicam was subsequently added to AgNDs/SiNWs materials for Raman detection. The lowest detected concentration of meloxicam was determined to be 0.1 μg/mL, and the linear range of meloxicam concentration was between 0.1 to 25 μg/mL (y=8.688 7x+89.945 9, R2=0.992 3) at the Raman peak intensity of 1 160 cm-1. Meloxicam in a compound capsule of anti-rheumatic Chinese patent medicine was further tested using the above mentioned method. Results showed that no meloxicam was detected in all of the samples. It was indicated that the concentration of meloxicam was less than 16.7 μg/g, far below the legal additional level of meloxicam (7.5 mg/g). The recovery rate of meloxicam was between 80.0% to 112.4%, which again proved the feasibility of the developed method in practical sample detection of meloxicam.

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龚娅军,姚卫蓉,谢云飞.表面增强拉曼光谱快速检测抗风湿类中成药中非法添加的美洛昔康[J].食品与生物技术学报,2021,40(6):42-51.

GONG Yajun, YAO Weirong, XIE Yunfei. Surface-Enhanced Raman Spectroscopy for Rapid Detection of Illegally Added Meloxicam in Anti-Rheumatic Chinese Patent Medicines[J]. Journal of Food Science and Biotechnology,2021,40(6):42-51.

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  • 在线发布日期: 2021-07-26
  • 出版日期: 2021-06-25
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