摘要
目的:建立禽畜肉中三甲胺的全自动顶空气相色谱-氮磷检测器测定方法。方法:称取禽肉样品10.000 g于50 mL离心管中,加入50 g·L^(-1)三氯乙酸溶液20 mL,匀浆仪均质2 min,4500 r·min^(-1)高速离心5 min,过滤,上清液过滤至50 mL容量瓶中,残渣再分别用25 mL的50 g·L^(-1)三氯乙酸分两次提取,滤液合并至容量瓶中,50 g·L三氯乙酸溶液定容。吸取提取液2.00 mL于顶空瓶中,压盖密封,用医用塑料注射器准确加入500 g·L^(-1)氢氧化钠溶液5.0 mL,全自动顶空进样,40℃平衡50 min,吸取顶空气体1.00 mL,进气相色谱分析,用HP-INNOWAX毛细管色谱柱程序升温,氮磷检测器分析,保留时间定性,外标法定量。结果:本试验方法测定禽畜肉中三甲胺的最低检出浓度为0.08 mg·kg^(-1),线性范围为0.10~10.00μg·mL^(-1),加标回收率可达90.2%~93.2%,批内精密度为4.67%~5.64%,批间精密度为4.77%~6.65%。结论:该方法具有全自动化程度高、操作简单快速、灵敏度高、准确度高以及重现性好等优点,适用于禽畜肉中三甲胺的测定。
Objective:A automatic headspace gas chromatography method with nitrogen phosphorus detector was developed for the determination of Trimethylamine(TMA)in domestic animal meat.Method:10.000 g prepared sample in 50 mL plastic centrifuge tube,adding 20 mL 50 g·L^(-1)trichloroacetic acid solution,homogenier for homogeneous 2 min 4500 r·min^(-1)centrifugation for 5 min,in the glass funnel with a little cotton,the supernatant into 50 mL volumetric flask,the residue was extracted with 25 mL trichloroacetic acid(50 g·L^(-1))for two times,and the filtrate was combined into a volumetric flask,and the 50 g·L^(-1)trichloroacetic acid solution was kept at constant volume.Accurately extract the extract 2.0 mL in headspace bottle,gland sealed,accurate injection of 5.0 mL 500 g·L^(-1)sodium hydroxide solution with medical plastic syringe.In automatic headspace sampler,the balance of 40℃ 50 min,1 mL from headspace gas analysis,gas chromatography,using HP-INNOWAX capillary column temperature programmed separation,analysis by nitrogen phosphorus detector,qualified by retention time and external standard method.Result:The minimum detectable concentration determination of trimethylamine in the livestock meat test method for 0.08 mg·kg^(-1),a linear range of 0.10~10.0μg·mL^(-1).The recovery rate can reach 90.2%~93.2%.The intra batch precision(RSD)was 4.67%~5.64%,and the inter batch precision was 4.77%~6.65%.Conclution:This method has a high degree of automation.The method is simple,rapid,sensitive,accurate and reproducible.It is suitable for the determination of trimethylamine in domestic animal meat.
作者
何漪
王韬
刘月月
朱莎
彭程
王勤
HE Yi;WANG Tao;LIU Yueyue;ZHU Sha;PENG Cheng;WANG Qin(Sanitary Inspection Department of Zibo Center for Disease Control and Prevention,Zibo 255026,China;Zibo Key Laboratory of Environmental Organic Pollution and Human Health Monitoring and Analysis,Zibo 255026,China)
出处
《食品安全导刊》
2022年第35期57-60,共4页
China Food Safety Magazine
基金
山东省医药卫生科技发展计划项目(202112010542)。
关键词
全自动
顶空
气相色谱法
三甲胺(TMA)
氮磷检测器
禽畜肉
automatic
headspaces
gas chromatography
trimethylamine(TMA)
nitrogen phosphorus detector
domestic animal meat
