CAJ | 학술논문

目的建立工作场所空气中氨基氰测定的高效液相色谱法.方法工作场所空气样品以水溶液作吸收液,用冲击式吸收管,以2.8～3.0 ml/min速度采集60 ain,以丹磺酰氯为衍生试剂,进行柱前衍生,衍生方法为待测样品中加入2.5 ml丙酮溶液,1.0 ml含0.016 mol/L碳酸钠和0.184 mol/L碳酸氢钠混合溶液,0.5 ml丹磺酰氯丙酮溶液(浓度为10 mg/ml),50℃水浴中反应1h.经色谱柱250 mm×4.6 mm×5 μm,ODS(C18)分离;流动相为乙腈-磷酸盐缓冲液(35:65);流速:1.0 ml/min,柱温25℃;荧光检测器检测,激发波长360 nm,发射波长495 nm.结果本法最低检出浓度为0.05 μg/ml,当氨基氰浓度为0.2～100.0 μg/ml呈良好线性关系,日内相对标准偏差0.28％～1.18％,日间相对标准偏差0.22％～2.16％;回收率95.7％～ 103.0％,采样效率为95.8％～96.9％.在避光条件下,氨基氰水溶液(pH＜6.5)常温可稳定7d.结论本方法稳定,可靠,操作方便,灵敏度高.适用于工作场所空气中氨基氰的测定.
목적 건립공작장소공기중안기청측정적고효액상색보법.방법 공작장소공기양품이수용액작흡수액,용충격식흡수관,이2.8～3.0 ml/min속도채집60 ain,이단광선록위연생시제,진행주전연생,연생방법위대측양품중가입2.5 ml병동용액,1.0 ml함0.016 mol/L탄산납화0.184 mol/L탄산경납혼합용액,0.5 ml단광선록병동용액(농도위10 mg/ml),50℃수욕중반응1h.경색보주250 mm×4.6 mm×5 μm,ODS(C18)분리;류동상위을정-린산염완충액(35:65);류속:1.0 ml/min,주온25℃;형광검측기검측,격발파장360 nm,발사파장495 nm.결과 본법최저검출농도위0.05 μg/ml,당안기청농도위0.2～100.0 μg/ml정량호선성관계,일내상대표준편차0.28％～1.18％,일간상대표준편차0.22％～2.16％;회수솔95.7％～ 103.0％,채양효솔위95.8％～96.9％.재피광조건하,안기청수용액(pH＜6.5)상온가은정7d.결론 본방법은정,가고,조작방편,령민도고.괄용우공작장소공기중안기청적측정.
Objective To establish a method for determining cyanamide in workplace air by highperformance liquid chromatography (HPLC).Methods Air samples were collected from the workplace using the shock absorption tube containing water solution at a rate of 2.8～3.0 ml/min for 60 min; dansyl chloride was used as a derivatization reagent to conduct pre-column derivatization,and the procedure was as follows:acetone solution (2.5 ml),mixed solution (1.0 ml) containing 0.016 mol/L Na2CO3 and 0.184 mol/L NaHC03,and 10 mg/ml acetone solution of dansyl chloride (0.5 ml) were added into the samples,and reaction proceeded in a water bath (50 ℃) for 1 h.HPLC was performed on an ODS C18 column (250 mm × 4.6 mm,5 μm) with a mobile phase of acetonitrile-phosphate buffer (35:65) at a flow rate of 1.0 ml/min and a column temperature of 25℃; a fluorescence detector was used at an excitation wavelength of 360 nm and an emission wavelength of 495 nm.Results The minimum detectable concentration of cyanamide was 0.05 μg/ml; a good linear relationship was noted when the concentration of cyanamide was 0.2～100.0 μg/ml; the intraday relative standard deviation (RSD) was 0.28％～1.18％,and the interday RSD was 0.22～2.16％; the recovery rate was 95.7％～ 103.0％,and the sampling efficiency was 95.8％～96.9％.Water solution of cyanamide (pH＜6.5) could be stable in the dark at room temperature for 7 d.Conclusion This method is stable,reliable,easy to operate,and highly sensitive and suitable for determination of cyanamide in workplace air.