基于SERS技术检测盐酸麻黄碱的研究

目的：建立盐酸麻黄碱的表面增强拉曼光谱（SERS）检测方法。方法：制备了银溶胶活性基底，并表征了其微观形态；对盐酸麻黄碱的拉曼峰进行了归属和指认，并对尿液中的样品进行了SERS检测；使用BWS415-785H型便携式拉曼光谱仪采集了拉曼光谱，其激发光源为785 nm，光谱测量范围为68~2 700 cm^-1，光谱分辨率小于3 cm^-1，激光功率为80 mW，积分时间为5 s。结果：确定了盐酸麻黄碱尿液中的检测下限为25 μg·mL^-1，曲线方程为Y=89.9X^0.7436（r²=0.992），平均回收率及其RSD分别为99.7%和6.2%。结论：该方法具有快速、准确、无损及操作简便等优点，为盐酸麻黄碱的现场快速检测打下了良好的基础。

Objective:To establish a method for the surface enhanced Raman spectroscopy(SERS)detection of ephedrine hydrochlorid. Methods:The active substrate of silver sol was prepared,and characterized by microscopic morphology. The Raman peaks of ephedrine hydrochloride were assigned,and the samples in urine were respectively detected by SERS. The Raman spectra were recorded by a portable laser Raman spectrometer BWS415-785H with a wavelength of 785 nm. The spectrometer provided that the spectral measurement range would be 68-2 700 cm^-1 and spectral resolution would be better than 3 cm^-1. The output power was maintained 80 mW in the experiment with 5 s of integration time. Results:The detection limit of urine of ephedrine hydrochloride was 25 μg·mL^-1,and the curve equation were Y=89.9X0.7436(r²=0.992). The average recovery rate and its RSD were 99.7% and 6.2%,respectively. Meanwhile,the SERS detection of the sample in urine verified the applicability of the method for detecting ephedrine hydrochloride. Conclusion:The method is fast,accurate,non-destructive and easy to operate,and it lays a good foundation for on-site rapid detection of ephedrine hydrochloride.

[1] 陆燕萍,刘佳丽,巩晓宇,等.麻黄药理作用及含量测定的研究进展[J].中国医药导报,2013,10(24):38 LU YP,LIU JL,GONG XY,et al.Research progress on the ephedra's pharmacological effects and its content determination[J].China Med Her,2013,10(24):38
[2] 刘桂红,乌英珍.禁毒工作中对含有麻黄碱成分易制毒药品的监管[J].中国人民公安大学学报(自然科学版),2016,89(3):64 LIU GH,WU YZ.Supervision of narcotics containing ephedrine in drug control work[J].J People Public Secur Univ China (Sci Technol),2016,89(3):64
[3] 刘旺培,马迅,刘小华,等.盐酸麻黄碱有关物质伪麻黄碱检查方法的改进[J].药物分析杂志,2015,35(7):1299 LIU WP,MA X,LIU XH,et al.Improvement of examination method for ephedrine hydrochloride related substances[J].Chin J Pharm Anal,2015,35(7):1299
[4] 王春雷,姜建伟,侯桂兰.急支糖浆HPLC特征指纹图谱研究及多成分定量测定[J].中草药,2016,47(23):4192 WANG CL,JIANG JW,HOU GL.Fingerprint and multi-components quantitative determination for Jizhi syrup by HPLC[J].Chin Tradit Herb Drugs,2016,47(23):4192
[5] 贺颖,王志萍,王力宁.HPLC法同时测定麻杏石甘汤剂中盐酸麻黄碱和苦杏仁苷含量[J].中华中医药杂志,2013,28(9):2778 HE Y,WANG ZP,WANG LN.HPLC simultaneous determination of ephedrine hydrochloride and amygdalin in Maxing Shigan decoction[J].China J Tradit Chin Med Pharm,2013,28(9):2778
[6] 黎春彤,李翔,马建丽,等.HPLC同时测定防风通圣丸中盐酸麻黄碱和盐酸伪麻黄碱的含量[J].药物分析杂志,2016,36(1):176 LI CT,LI X,MA JL,et al.Simultaneous determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Fangfeng Tongsheng pills by HPLC[J].Chin J Pharm Anal,2016,36(1):176
[7] 洪美华,卓小萍,何世柯,等.小儿咳喘灵颗粒中盐酸麻黄碱含量测定的2种HPLC法比较[J].中国药房,2008,27(12):2122 HONG MH,ZHUO XP,HE SK,et al.Determination of ephedrine hydrochloride in Xiaoer Kechuanling granules by two different HPLC methods:a contrastive analysis[J].China Pharm,2008,27(12):2122
[8] 王乐.GC-MS法分析检验麻黄碱[D].兰州:甘肃政法学院,2015 WANG L.The Study on the Determination of Ephedrine by GC-MS[D].Lanzhou:Gansu Institute of Political Science and Law,2015
[9] 李宁,宋玉乔,吕效兴,等.LC-MS/MS法快速测定人血浆中盐酸伪麻黄碱的血药浓度[J].现代科学仪器,2008,18(3):53 LI N,SONG YQ,LÜ XX,et al.LC-MS/MS fast determination of the drug concentration of pseudo-ephedrine hydrochloride in human plasma[J].Mod Sci Instrum,2008,18(3):53
[10] 臧永丽,高慧菊.麻黄碱的TLG-SERS研究[J].聊城师院学报(自然科学版),2000,13(2):57 ZANG YL,GAO HJ.TLG-SERS study on ephedrine[J].J Liaocheng Teach Univ(Nat Sci),2000,13(2):57
[11] HAN Z,LIU H,WANG B,et al.Three-dimensional surface-enhanced Raman scattering hotspots in spherical colloidal superstructure for identification and detection of drugs in human urine[J].Anal Chem,2015,87(9):4821
[12] QIN YQ,JI XH,JING J,et al.Size control over spherical silver nanoparticles by ascorbic acid reduction[J].Colloids Surf A Physicochem Eng Asp,2010,372(1-3):172
[13] 林翔.SERS基底的制备及其用于食品中污染物的快速检测[D].哈尔滨:哈尔滨工业大学,2016 LIN X.Fabrication of SERS Platforms and ITS Application on Fast Detection of Food Contaminants[D].Harbin:Harbin Institute of Technology,2016
[14] JANA NR,PAL T.Anisotropic metal nanoparticles for use as surface-enhanced Raman substrates[J].Adv Mater,2007,19(13):1761
[15] 陈志俊,赵航,包琳,等.基于表面增强拉曼光谱技术检测阿斯巴甜[J].光散射学报,2018,30(1):28 CHEN ZJ,ZHAO H,BAO L,et al.Detection of aspartame based on the surface-enhanced Raman spectroscopy[J].Chin J Light Scat,2018,30(1):28
[16] ZHAO H,HASI WLJ,BAO L,et al.Rapid detection of sildenafil drugs in liquid nutraceuticals based on surface-enhanced Raman spectroscopy technology[J].Chin J Chem,2017,35(10):1522
[17] 中华人民共和国药典2015年版.二部[S].2015:1076 ChP 2015.Vol Ⅱ[S].2015:1076