GC-MS-相转移衍生化法分析水相中亚硝酸根离子

DETERMINATION OF NITRITE IN AQUEOUS SAMPLES BY PHASE-TRANSFER CATALYZED DERIVATIZATION AND GAS CHROMATOGRAPHY-MASS SPECTROMETRY

采用相转移催化剂四辛基溴化铵及五氟苄基溴将水相(血、尿)中亚硝酸根离子衍生化生成可挥发性化合物,然后用GC-MS法进行测定。亚硝酸根离子含量在0.2～10μg/mL范围内与离子峰面积呈良好的线性关系,相关系数r=0.9998,检出限为0.1μg/mL。用该方法对水、尿、血中亚硝酸根离子进行测定,测定结果的相对标准偏差为1.44%～4.17%(n=6),回收率为82%～84%。

The GC - MS method for detection of nitrite from aqueous samples was established. The nitrite in aqueous samples （blood, urine） derivatized with tetraoctylammonium bromide to volatile stable compound, pentafluorobenzyl bromide as catalysts. In the range of 0.2 - 10 μg/mL, nitrite concentration was linear with ion peak area and the linear relative coefficient was 0.999 8. The detection limit was 0.1 μg/mL. The method was applied to detect water, urine and blood plasma samples. The RSD of detection results was 1.44% -4.17% （n =6） and the recovery was 82% -84%.