GC-FID法同时测定腌制鱼干中9种N-亚硝胺类化合物
Simultaneous Determination of Nine N-nitrosamine in Pickling Dried Fish by GC-FID
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摘要: 在气相色谱-氢火焰检测器的基础上建立了同时测定腌制鱼干中9种N-亚硝胺类化合物的方法。采用碱液加热处理结合二氯甲烷萃取的方法提取腌制鱼干的N-亚硝胺,经棷壳活性炭净化,C18固相萃取(SPE,Solid Phase extraction)小柱富集,样液用DB-WAXETR极性柱(30 m×0.25 mm,0.25 μm)进行色谱分离,柱温采用程序升温。结果显示:该方法下的9种N-亚硝胺类化合物在0.05~5 μg/mL浓度范围内线性良好(R2＞0. 999);检出限和定量限范围分别为0.05~0.29 μg/mL和0.18~0.95 μg/mL;回收率和RSD分别为76.8%~129.5%和2.29%~15.5%。对市售的50种腌制鱼干进行检测,N-亚硝基二乙胺(NDEA,N-nitrosodiethylamine)、N-亚硝基哌啶(NDIP,N-Nitrosopiperidine)N-亚硝基吡咯烷(NPYR,N-Nitrosopyrrolidine)检出率分别达到20%、20%、24%,只有一种样品的N-亚硝基二甲胺(NDMA,N-nitrosodimethylamine)超过国标限量规定(4 μg/kg)。Abstract: A method for the simultaneous determination of nine N-nitrosamine in pickling dried fish was developed by gas chromatography-hydrogen flame detector(GC-FID)with by lye heating treatment combined with dichloromethane extraction. The filtrate was purified by coconut shell activated carbon,and concentrated by C18 SPE columns;the chromatographic separation were carried with a DB-WAXETR polar column(30 m×0.25 mm,0.25 μm). The column temperature was programmed to rise. Results showed that:The Nine nitrosamines had good linearity in the range of 0.05~5 μg/mL(R2>0. 999);The detection limits and quantitation limits were ranged from 0.05 to 0.29 μg/mL and 0.18 to 0.95 μg/mL. The recoveries and RSD were 76.8%~129.5% and 2.29%~15.5%. The actual sample detection result in 50 kinds of pickled dried fish showed that the detection rates of NDEA,NDIP and NPYR were 20%,20% and 24%. Only one sample exceeded the national standard limit(NDMA<4 μg/kg).
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