胃液中挥发性亚硝胺含量的气相色谱/热能分析仪测定

Determination of volatile nitrosamines in gastric juice by GC-TEA

目的:建立胃液中挥发性亚硝胺含量测定方法。方法:采用气相色谱/热能分析仪联用,内标物为对亚硝基二苯胺;色谱条件为玻璃柱2m×2mm(ID),固定相为10%(w/w)Carbowax×20M/Chromosorb WHP(80～100目);进样口温度220℃;柱温100℃(保持1min),以10℃/min升到150℃(保持2min),然后以2℃/min升到190℃;裂解温度550℃;接口温度275℃;反应室真空度38.38kPa;载气氮气,流速25mL/min。测定河南林县313名居民胃液中挥发性亚硝胺(二甲基亚硝胺(NDMA)、二乙基亚硝胺(NDEA)、甲基苄基亚硝胺(NMBzA)、亚硝基吡咯烷(NPYR)、亚硝基哌啶(NPIP))的含量。结果及结论:该方法简单、快速、重现性好。线性关系良好,平均加样回收率NDMA92.50%,RSD=3.2%;NDEA95.34%,RSD=2.8%;NMBzA95.24%,RSD=3.0%;NPYR93.04%,RSD=3.1%;NPIP90.53%,RSD=3.6%。

Aim： To establish a method for the determination of volatile nitrosamines in gastric juice. Methods：GC-TEA was connected, with NDPA as internal standard; analysis was carried out on 2 m × 2 mm （ID） glass column with 10% Carbowax × 20 M/Chromosorb WHP（80 - 100 mesh） ; injection temperature： 220 ℃ ; oven temperature： 100 ℃ （1 min） ,10 ℃/min to 150 ℃ （2 min） , 2 ℃/min to 190 ℃ ; split temperature： 550 ℃ ; mouthpiece temperature： 275 ℃ ; vacuity of reaction：38.38 kPa; carrier gas： N2, flow rate：25 ml/min. Volatile nitrosamines （NDMA, NDEA, NMBzA, NPYR, and NPIP） in gastric juice of residents in Linzhou city, Henan province were determined by GC-TEA. Results and Conclusion： It reveals that the method is simple, rapid and reproducible with a good linear relationship. The average recovery was NDMA：92.50% ,RSD = 3.2% ;NDEA：95.34% , RSD = 2.8% ; NMBzA：95.24% , RSD = 3.0% ;NPYR：93.04% ,RSD =3.1% ;NPIP：90.53% ,RSD =3.6%.