王超洋, 秦文华, 耿琪. 正交法优化顶空-气相色谱法测定血中氯丁二烯的实验条件[J]. 环境与职业医学, 2016, 33(1): 69-72. DOI: 10.13213/j.cnki.jeom.2016.15235
引用本文: 王超洋, 秦文华, 耿琪. 正交法优化顶空-气相色谱法测定血中氯丁二烯的实验条件[J]. 环境与职业医学, 2016, 33(1): 69-72. DOI: 10.13213/j.cnki.jeom.2016.15235
WANG Chao-yang, QIN Wen-hua, GENG Qi. Using Orthogonal Experimental Design to Explore Optimal Experimental Conditions for Determination of Chloroprene in Blood by Headspace Gas Chromatography[J]. Journal of Environmental and Occupational Medicine, 2016, 33(1): 69-72. DOI: 10.13213/j.cnki.jeom.2016.15235
Citation: WANG Chao-yang, QIN Wen-hua, GENG Qi. Using Orthogonal Experimental Design to Explore Optimal Experimental Conditions for Determination of Chloroprene in Blood by Headspace Gas Chromatography[J]. Journal of Environmental and Occupational Medicine, 2016, 33(1): 69-72. DOI: 10.13213/j.cnki.jeom.2016.15235

正交法优化顶空-气相色谱法测定血中氯丁二烯的实验条件

Using Orthogonal Experimental Design to Explore Optimal Experimental Conditions for Determination of Chloroprene in Blood by Headspace Gas Chromatography

  • 摘要: 目的

    探索顶空-气相色谱法测定血中氯丁二烯的最优实验条件。

    方法

    利用正交设计方法,顶空进样器和气相色谱仪分别选用L32(49)和L16(45)正交表进行实验,并用极差分析法和综合平衡法统计结果。

    结果

    最优水平组合为,顶空进样器:样品体积5.0 mL、炉温65℃、取样针温75℃、传输线温115℃、保温时间25 min、进样时间0.04 min、加压时间1.5 min、拔针时间0.2 min、柱压22 psi;气相色谱仪:进样口温度210℃、柱箱温度40℃、检测器温度370℃、载气流速1.6 mL/min、分流比5:1。该条件下工作曲线为ŷ=3 315.5x+6 340.3,r=0.999 8,检测限为0.10 μg/L。

    结论

    正交设计用于探索顶空-气相色谱法测定血中氯丁二烯的最优实验条件,可减少实验的盲目性,提高准确性。

     

    Abstract: Objective

    To explore the optimal experimental conditions for determination of chloroprene in blood by headspace gas chromatography.

    Methods

    Two orthogonal arrays were used to design two key experimental matrices, specifically L32 (49) for headspace sampler and L16 (45) for gas chromatography. Results were analyzed by range analysis and comprehensive balance method.

    Results

    The optimal experimental conditions of headspace sampler were as follows:sample volume of 5.0 mL; furnace temperature at 65℃; sampling needle temperature at 75℃; transfer line temperature at 115℃; holding time for 25 min; injection time for 0.04 min; pressure time for 1.5 min; extraction time for 0.2 min; column pressure at 22 psi. The optimal experimental conditions of gas chromatography were as follows:inlet temperature at 210℃; column temperature at 40℃; detector temperature at 370℃; flow rate of carrier gas at 1.6 mL/min; split ratio of 5:1. Under above conditions, the working curve was ŷ=3 315.5x+6 340.3, with a correlation coefficient (r)=0.999 8, and the detection limit was 0.10 μg/L.

    Conclusion

    Using the orthogonal experimental method to explore the optimal experimental conditions for determination of chloroprene in blood by headspace gas chromatography could reduce blindness and increase accuracy.

     

/

返回文章
返回