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

[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 m L、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 m L/min、分流比5∶1。该条件下工作曲线为?=3 315.5x+6 340.3,r=0.999 8,检测限为0.10μg/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。

[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 （4^9） for headspace sampler and L16 （4^5） 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 y=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.