摘要
在海藻食品中总砷含量分析过程中,砷离子形态不稳定,会干扰总砷检测结果。为此,开展了气相色谱-串联质谱法测定海藻食品中总砷的研究。使用4.0 mL硝酸和1.5 mL过氧化氢溶液对海藻食品样品进行微波消解,赶酸阶段加入不同配比的正己烷和乙酸酐混合洗脱剂。经超纯水定容后,获得的海藻食品样品衍生物用于气相色谱仪和质谱仪的检测。结果表明:在气相色谱仪的SCAN模式下,100.0μL正己烷+200.0μL乙酸酐洗脱剂组对应的AsB、DMA、As(Ⅲ)、MMA以及As(Ⅴ)色谱峰分离效果最佳,即定性分析最准确。质谱仪在Auto SRM模式下的定量检测结果显示,载气流量1.05 mL/min与补气流量0.45 mL/min组合下,检测结果最为精确;所提方法的回收率为96.0%~97.0%,且与标准方法测定结果基本一致,偏差<2%。优化洗脱剂的配比,以及合理设置载气流量和补气流量,可确保砷离子形态的稳定,从而获得准确的含量检测结果。
During the analysis of total arsenic content in seaweed food,the unstable ion form of arsenic itself can interfere with the detection results.Therefore,a study was conducted on the determination of total arsenic content in seaweed food by gas chromatography-tandem mass spectrometry.Microwave digestion of seaweed food samples was performed using 4.0 mL nitric acid and 1.5 mL hydrogen peroxide solution.Different ratios of n-hexane and acetic anhydride mixed eluents were added during the acid removal stage.After being diluted with ultrapure water,the derivatives of seaweed food samples obtained are used for detection by gas chromatography and mass spectrometry.The results showed that in the SCAN mode of the gas chromatograph,the 100.0μL n-hexane and 200.0μL acetic anhydride eluent group achieved optimal chromatographic peak separation for AsB,DMA,As(III),MMA,and As(V),indicating the most accurate qualitative analysis.The quantitative detection results of the mass spectrometer in Auto SRM mode showed that the combination of carrier gas flow rate of 1.05 mL/min and make-up gas flow rate of 0.45 mL/min yielded the most accurate detection results;The proposed method has a detection recovery rate between 96.0%and 97.0%,which is basically consistent with the results obtained by the standard method,with a deviation within 2%.Proper use of eluent,as well as reasonable settings of carrier gas flow rate and replenishment gas flow rate,can ensure the stability of arsenic ion forms and obtain accurate content detection results.
作者
汤浩源
TANG Hao-yuan(Comprehensive Supervision and Law Enforcement Bureau,Shibei District Health Bureau of Qingdao City,Qingdao 266000,China)
出处
《粮食与饲料工业》
2025年第4期126-130,共5页
Cereal & Feed Industry
关键词
气相色谱-串联质谱法
海藻食品
砷含量
微波消解
洗脱剂
色谱峰分离
定性分析
定量检测
gas chromatography-tandem mass spectrometry
seaweed food
arsenic content
microwave digestion
eluent
chromatographic peak separation
qualitative analysis
quantitative detection
