基于Au@Ag纳米粒子的表面增强拉曼光谱技术测定苹果和梨中的福美双

Determination of thiram in apples and pears by surface enhanced Raman spectroscopy based on Au@Ag nanoparticles

中文关键词:  Au@Ag纳米粒子  表面增强拉曼光谱  苹果  梨  福美双

英文关键词:Au@Ag nanoparticles  surface enhanced Raman spectroscopy  apples  pears  thiram

中文摘要:

      目的 建立基于Au@Ag纳米粒子(Au@Ag nanoparticles, Au@AgNPs)的表面增强拉曼光谱(surface enhanced Raman spectroscopy, SERS)测定苹果和梨中的福美双的方法。方法 采用快速、简便、廉价、有效、坚固、安全(QuEChERS)样品制备方法提取苹果和梨中的福美双, 提取液直接与Au@AgNPs结合后进行SERS测试。DXRxi-Raman激光拉曼光谱仪条件: 激发波长532 nm±0.5 nm, 光谱覆盖范围300~1700 cm-1, 光谱分辨率为2~5 cm-1, 最后采用超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)进行验证。结果 拉曼位移为1379 cm-1处的特征峰可以作为福美双残留检测的拉曼特征峰, 待测样品和Au@AgNPs加入量分别为20 μL和10 μL, 吸附时间为5 min时, 苹果中福美双的检出限能达到0.1 mg/kg, 相关系数为0.9942, 相对标准偏差为5.21%~6.11%, 回收率为90.0%~98.0%; 梨当中福美双的检出限能达到0.1 mg/kg, 相关系数为0.9924, 相对标准偏差为4.21%~5.11%, 回收率为92.0%~98.4%。与UPLC-MS/MS的对比结果具有较好的一致性。结论 该方法具有操作简单、快速、准确等优点, 可适用于苹果和梨中福美双的检测分析。

英文摘要:

      Objective To establish a method for the rapid detection of thiram in apples and pears by surface enhanced Raman spectroscopy (SERS) method based Au@Ag nanoparticles (Au@AgNPs). Methods The quick easy cheap effective rugged and safe (QuEChERS) sample preparation method was used to extract thiram in apples and pears, and the extract solution was directly combined with Au@AgNPs for SERS test. DXRxi-Raman laser Raman spectrometer test conditions as follows: The excitation wavelength of the experiment was 532 nm±0.5 nm, the spectral coverage was 300?1700 cm-1, and the spectral resolution was 2-5 cm-1, and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used for verification finally. Results The characteristic peak at the Raman shift of 1379 cm-1 can be used as the Raman peak for the detection of thiram residues. The amount of the sample to be tested and Au@AgNPs were 20 μL and 10 μL, respectively, and the adsorption time was 5 min. The limit of detection for thiram in apples was 0.1 mg/kg, the r2 and the relative standard deviations were 0.9942, 5.21%?6.11%, respectively, the recoveries were 90.0%-98.0%; the limit of detection for thiram in pears was 0.1 mg/kg, the r2 and the relative standard deviations were 0.9924, 4.21%?5.11%, respectively, the recoveries were 92.0%?98.4%. These results were in good agreement with the UPLC-MS/MS. Conclusion This method is simple, rapid and accurate, and can be applied to the detection and analysis of thiram in apples and pears.