银纳米溶胶表面增强拉曼光谱法快速测定鱼腥草注射液中依诺沙星的含量  

Rapid Determination of Enoxacin in Herba Houttuyniae Injection by Surface-Enhanced Raman Spectroscopy with Silver Nanosol

作　　者：陈美芳 王鑫 陈宏炬 艾连峰 马莉[1] CHEN Meifang;WANG Xin;CHEN Hongju;AI Lianfeng;MA Li(Hebei Key Laboratory of Environment and Human Health,School of Public Health,Hebei Medical University,Shijiazhuang 050017,China;Xiamen Pers Nano Technology Limited Company,Xiamen 361000,China;Shijiazhuang Customs Technology Center,Shijiazhuang 050057,China)

机构地区：[1]河北医科大学公共卫生学院河北省环境与人群健康重点实验室,石家庄050017 [2]厦门普识纳米科技有限公司,厦门361000 [3]石家庄海关技术中心,石家庄050057

出　　处：《理化检验（化学分册）》2024年第12期1263-1268,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：河北省自然科学基金面上项目(H2021206245);国家自然科学基金面上项目(82173576);河北省重点研发计划项目-农业高质量发展关键共性技术攻关专项(21326616D)。

摘　　要：以自制银纳米溶胶为基底,采用表面增强拉曼光谱法(SERS)快速测定鱼腥草注射液中依诺沙星的含量。取1 mL质量分数1%的硝酸银溶液置于烧杯中,加入200 mL水,以转速8 000 r·min^(-1)搅拌,并加热至沸腾,逐滴加入9 mL质量分数1%的柠檬酸钠溶液至溶液变为黄色,继续煮沸直至溶液变为乳白色,停止加热,冷却至室温,以转速3 000 r·min^(-1)离心1 min,收集40 mL上层液体于离心管,加入5 mL水,以转速5 000 r·min^(-1)离心5 min,弃去上清液,再加入5 mL水并超声5 min,所得的银纳米溶胶于4℃储存。取0.2 mL样品,加入0.1 mL银纳米溶胶,利用拉曼光谱仪在200~3 200 cm^(-1)内进行检测。结果表明,依诺沙星的质量浓度在0.5~100 mg·L^(-1)内在1 469 cm^(-1)拉曼位移处对应的响应强度呈线性关系,检出限(3S/N)为0.043 mg·L^(-1);对空白样品进行3个浓度水平的加标回收试验,回收率为86.1%~103%,测定值的相对标准偏差(n=5)为3.0%~5.7%。Using the self-made silver nanosol as the substrate,the method for rapid determination of enoxacin in Herba Houttuyniae injection by surface-enhanced Raman spectroscopy with silver nanosol was proposed.1 mL of 1%(mass fraction)silver nitrate solution was taken and placed in a beaker,and 200 mL of water was added.The mixture was mixed at a rotational speed of 8000 r·min^(-1) and heated to boiling.9 mL of 1%(mass fraction)sodium citrate solution was added dropwise until the solution turned yellow,and the heating was stopped until the solution turned milky white.The solution was cooled to room temperature,and centrifuged at a rotational speed of 3000 r·min^(-1) for 1 min.The upper solution(40 mL)was collected into the centrifuge tube,and 5 mL of water was added.The solution was centrifuged at a rotational speed of 5000 r·min^(-1) for 5 min,and the supernatant was discarded.5 mL of water was added,and the mixture was ultrasonic treated for 5 min.The resulting silver nanosol was stored at 4℃.The 0.2 mL of sample was taken,and 0.1 mL of silver nanosol was added.The mixture was detected within 200-3200 cm^(-1) using Raman spectrometer.As shown by the results,linear relationship between the corresponding response intensity at Raman shift of 1469 cm^(-1) and mass concentration of enoxacin was found in the range of 0.5-100 mg·L^(-1),with detection limit(3S/N)of 0.043 mg·L^(-1).Test for recovery was made on blank sample by standard addition method at 3 concentration levels,giving results in the range of 86.1%-103%,with RSDs(n=5)of the determined values in the range of 3.0%-5.7%.

关 键 词：表面增强拉曼光谱法(SERS) 银纳米溶胶 鱼腥草注射液 依诺沙星 

分 类 号：O657.37[理学—分析化学]