Fan Jiahua, Cai Ying, Yan Zhihong, Li Yang, Yao Xuelian
College of pharmacy, Jiangxi University of Chinese Medicine, Nanchang 330004, China.
College of pharmacy, Jiangxi University of Chinese Medicine, Nanchang 330004, China.
J Chromatogr A. 2023 Apr 12;1694:463904. doi: 10.1016/j.chroma.2023.463904. Epub 2023 Feb 27.
Graphene-functionalized nickel foam (NF) sorbent materials were prepared and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy and Thermogravimetric analysis. For the separation and detection of polycyclic aromatic hydrocarbons (PAHs) in five Chinese medicine samples, namely dandelion, fructus aurantii, peppermint, mulberry leaf and embryo chrysanthemum, a method combining dispersive micro-solid phase extraction and gas chromatography-mass spectrometry (GC-MS) was developed. Four conditions affecting the extraction efficiency, such as the type of desorption solvent, the amount of sorbent, the extraction time and the volume of water sample, were optimized. The results of the methodological validation showed that NF@SiO@G was able to adsorb PAHs well and with good reproducibility. All analytes showed good linearity in the concentration range of 20-2000 ng/mL with coefficient of determination R≥0.9956. The limit of detection was 0.98-13.34 ng/mL, and the limit of quantification ranged from 3.25 to 44.47 ng/mL. Both the intra-day and inter-day precision were lower than 15.46%, and the spiked recoveries were in the range of 75.5-118.4%. The total contents of the 16 PAHs contained in these five Chinese herbal medicines (CHMs) were varied from 450 to 1557 µg/kg. The results indicated that the graphene-functionalized NF sorbent combined with GC-MS can effectively detect PAHs in CHMs.
制备了石墨烯功能化泡沫镍（NF）吸附剂材料，并通过扫描电子显微镜、傅里叶变换红外光谱、X射线衍射、X射线光电子能谱和热重分析对其进行了表征。为了分离和检测五种中药样品（即蒲公英、枳壳、薄荷、桑叶和杭白菊）中的多环芳烃（PAHs），开发了一种分散微固相萃取与气相色谱-质谱联用（GC-MS）的方法。优化了影响萃取效率的四个条件，如解吸溶剂类型、吸附剂用量、萃取时间和水样体积。方法学验证结果表明，NF@SiO@G能够很好地吸附PAHs，且重现性良好。所有分析物在20-2000 ng/mL浓度范围内均表现出良好的线性，决定系数R≥0.9956。检测限为0.98-13.34 ng/mL，定量限为3.25-44.47 ng/mL。日内和日间精密度均低于15.46%，加标回收率在75.5%-118.4%范围内。这五种中药材（CHMs）中所含16种PAHs的总含量在450-1557 μg/kg之间。结果表明，石墨烯功能化NF吸附剂与GC-MS联用能够有效检测中药材中的PAHs。
