CAJ | 학술논문

建立了金属络合衍生和反相高效液相色谱检测主流烟气中氰化氢的方法.该方法以Ni(II)-NH3为金属络合衍生化试剂,以5 mmol/L四戊基溴化铵为离子对试剂,分析时间小于10 min.氰化物标准工作曲线在0.1~20μg/mL范围内线性关系良好(R2>0.999);检出限和定量限分别为0.049和0.162μg/支;3个加标水平回收率在87.41% ~ 119.47%.该法与连续流动法测定结果较为一致:肯塔基对照卷烟 3R4F 检测结果相对偏差为-5.35%,15 种卷烟样品测定结果相对偏差在-0.79%~ 8.51%.
건립료금속락합연생화반상고효액상색보검측주류연기중청화경적방법.해방법이Ni(II)-NH3위금속락합연생화시제,이5 mmol/L사무기추화안위리자대시제,분석시간소우10 min.청화물표준공작곡선재0.1~20μg/mL범위내선성관계량호(R2>0.999);검출한화정량한분별위0.049화0.162μg/지;3개가표수평회수솔재87.41% ~ 119.47%.해법여련속류동법측정결과교위일치:긍탑기대조권연 3R4F 검측결과상대편차위-5.35%,15 충권연양품측정결과상대편차재-0.79%~ 8.51%.
A reverse phase high performance liquid chromatography method was developed for determination of hydrogen cyanide in cigarette mainstream smoke via metal-complexing derivatization. By using Ni(Ⅱ)-NH3 as derivatizating agent, the proposed method can achieve the analysis within 10 minutes using 5 mmol/L tetraamylammonium bromide as ion-pair reagent. The method enabled good linearity in the range from 0.1 to 20μg/mL for the standard working solutions withR2 higher than 0.999. The limit of detection and limit of quantization were 0.049μg/cig and 0.162μg/cig, respectively. The recoveries for spiked samples at three levels were between 87.41% and 119.47%. The test results of the proposed method were in good agreement with that of continuous flow method with a relative deviation of -5.35% for Kentucky reference cigarette 3R4F and a relative deviation range from -0.79% to 8.51% for 15 cigarette samples.