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    顶空-箭形固相微萃取-气相色谱-质谱法测定水中松节油的含量

    Determination of Turpentine in Water by GC-MS after Headspace and Solid Phase Micro-Extraction Arrow

    • 摘要: 在顶空瓶中加入水样10.0 mL、氯化钠3 g和20.0 mg·L-1内标溶液10.0 μL,选择涂层为120 μm二乙烯苯/聚二甲基硅氧烷的箭形固相微萃取头,于50℃萃取30 min,脱附的气体用DB-1毛细管色谱柱分离,质谱仪检测,内标法定量。结果显示:松节油的主要成分为α-蒎烯,还有少量莰烯、β-蒎烯和柠檬烯等;松节油标准曲线的线性范围为5.0~100.0 μg·L-1,检出限(3.143s)为0.6 μg·L-1;对空白样品进行加标回收试验,回收率为95.9%~98.0%,测定值的相对标准偏差(n=6)为3.7%~4.3%;方法用于实际样品分析,结果均未检出松节油。

       

      Abstract: 10.0 mL of the water sample, 3 g of sodium chloride and 10.0 μL of 20.0 mg·L-1 internal standard solution were added into headspace flask and extracted at 50℃ for 30 min with solid phase micro-extraction arrow head coated with 120 μm divinylbenzene/polydimethylsiloxane. The desorbed gas was separated on DB-1 capillary column, detected by mass spectrometer, and quantified by internal standard method. It was shown that the main component of turpentine was α-pinene, with small amounts of camphene, β-pinene and limonene, and the linear range of standard curve of turpentine was 5.0-100.0 μg·L-1, with detection limit (3.143s) of 0.6 μg·L-1. Test for recovery was made on the blank sample by standard addition method, giving results in the range of 95.9%-98.0%, and RSDs (n=6) of the determined values were ranged from 3.7% to 4.3%. This method was applied to analysis of the actual samples, and turpentine was not detected.

       

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