新型固相微萃取涂层材料的制备及其在迷迭香挥发性成分检测分析中的应用

利用溶胶-凝胶法制备了含全羟基取代五元瓜环(Q[5])的新型固相微萃取涂层。以全羟基取代五元瓜环(Q[5](OH)_(10))和端羟基聚二甲基硅氧烷(OH-PDMS)为起始原料,γ-缩水甘油醚氧丙基三甲氧基硅烷(KH-560)为偶联试剂,通过水解和缩合反应制备了PDMS/Q[5](OH)_(10)新型涂层。采用扫描电镜、傅立叶红外光谱、差示扫描量热分析和热重分析分别对涂层组织形貌、结构特点以及热稳定性进行了检测。结果表明该涂层具有较大的表面积,良好的热稳定性(360℃)和较长的使用寿命。将该涂层制备成固相微萃取纤维,联用气相色谱-质谱技术对迷迭香的挥发性成分进行了分析,并用面积归一法测定其相对含量。优化的萃取条件为:萃取温度80℃,萃取时间45 min,样品质量0.200 0 g。在此条件下,鉴定出迷迭香中的25种挥发性成分,含量较高的成分为1,8-桉叶素、樟脑和α-蒎烯。将自制纤维与商用纤维(PDMS/DVB/CAR)的萃取效果进行了对比,从萃取成分的数量和含量来看,自制纤维的萃取效果和商用纤维相当,说明自制的固相微萃取纤维可用于植物中挥发性成分的快速检测分析。

Preparation of a Novel Solid-phase Microextraction Coating and Its Application in Determination of Volatile Components in Rosmarinus officinalis L.

A novel solid phase microextraction coating that contains perhydroxy cucurbit [5] uril was prepared by a sol-gel method.With 3-(2-cyclooxypropoxyl) propyltrimethoxysilane as cross-linking agent,Perhydroxyl cucurbit [5] uril (Q [5] (OH) 10) and hydroxy-terminated poly (dimethylsiloxane) (OH-PDMS) were used as starting coating material to bond chemically to a fused-silica substrate to form a PDMS/Q [5] (OH)10 coating by hydrolysis and polycondensation reactions.The surface morphology,microstructure and thermal stability of the obtained composite coating were characterized by scanning electron microscopy (SEM),Fourier-transform infrared spectrometry(FTIR),differential scanning calorimetry (DSC) and thermogravimetric (TG) analysis.The results showed that the coating has a large specific surface area,high thermal stability (360 ℃) and long lifetime.Its performance was tested using a homemade solid-phase microextraction coating fiber coupled with gas chromatography-mass spectrometry (GC-MS) to analyze volatile components in Rosmarinus officinalis L(ROL).The optimized solid-phase microextraction conditions included an extraction temperature of 80 ℃,an extraction time of 45 min and a 0.200 0 g sample.The volatile components were extracted by head solid-phase microextraction(HS-SPME) with a homemade extraction fiber,and identified by GC-MS.The relative content of each component was determined by area normalization.Twenty-five compounds in the ROL were identified.The main compounds are 1,8-cineole,camphor and α-pinene.The homemade fiber was compared with commercial fiber (PDMS/DVB/CAR).According to the quantity and content of the extracts from ROL,the extraction effect of the two kinds of fiber are equivalent,which indicated that the homemade novel fiber could be applied in the rapid detection of volatile components in plants.