摘要
建立了超声辅助提取,气相分子吸收光谱法测定火腿中亚硝酸盐含量的高效、高灵敏分析方法。采用纯水提取火腿中的亚硝酸盐,对室温提取、水浴热提法和超声辅助提取法对火腿中亚硝酸盐的提取效率进行了比较。结果表明:超声辅助提取法对火腿中亚硝酸盐的提取效率最佳。探究了超声提取时间及提取温度对火腿中亚硝酸盐提取的影响,结果表明:采用该法在60℃下,30 min内,可以实现对火腿中亚硝酸盐的充分和稳定性提取。在优化的实验条件下,本方法应用于火腿中亚硝酸盐含量的测定,方法检出限为44.0μg/kg(以NO_(2)-N计);对实际火腿样品中亚硝酸盐的5次重复测试的相对标准偏差为3.1%;回收率在87.7%-111.6%之间。该方法准确可靠,较之传统离子色谱法及分光光度法,本法兼具灵敏和快速的优势,可以在火腿中亚硝酸盐检测领域推广应用。
A sensitive and high performance method was established for the determination of nitrite in hams by gas phase molecular absorption spectrometry.Nitrite in ham samples was extracted with water and the extraction efficiency was validated based on room-temperature extraction,hot water-bath leaching and ultrasonic extraction,respectively.Generally,as showed in the results,better extraction efficiency and precision were acquired using the ultrasonic extraction method.Furthermore,the extraction time and temperature influencing the extraction result were optimized and the results exhibited that nitrite in hams could be adequately and stably extracted within 30 min under the extraction temperature of 60℃.Under the optimized conditions,the limit of determination for the method was 44.0μg/kg as NO_(2)-N,and the relative standard deviation based on 5 duplicate tests of nitrite in real ham samples was 3.1%,and the recoveries were in the range of 88.7%-111.6%,which showed that the method was accurate and reliable.Compared with the traditional ion chromatography and spectrophotometric methods,this method had the both merits of low detecting limit and high performance.Therefore,it was feasible for the application and popularization in detection of nitrite in hams.
作者
刘丰奎
汪雨
钱春燕
李杰
姜雪成
邵鹏
祖文川
LIU Fengkui;WANG Yu;QIAN Chunyan;LI Jie;JIANG Xuecheng;SHAO Peng;ZU Wenchuan(School of Precision Instrument and Opto-electronics Engineering,Tianjin University,Tianjin 300072;Beijing Center for Physical&Chemical Analysis,Beijing 100089;Shanghai Institute of Measurement and Testing Technology,Shanghai 201203)
出处
《分析科学学报》
CAS
CSCD
北大核心
2022年第1期89-93,共5页
Journal of Analytical Science
基金
国家重点研发计划(No.2018YFF010117004)
北京科学技术研究院改革与发展经费培育类项目(No.PY2020HJ36)
北京市科技计划(No.Z201100009319001)。
关键词
气相分子吸收光谱法
超声辅助提取
亚硝酸盐
火腿
Gas phase molecular absorption spectrometry
Ultrasonic assisted extraction
Nitrite
Hams
