程序升温大体积进样在HRGC-HRMS法测定食品中PCDD/F的应用  

Determination of PCDD/Fs in food samples using programmable temperature vaporizer-based large volume injection by high resolution gas chromatography-high resolution mass spectrometry

作　　者：张磊[1] 李敬光[1] 赵云峰[1] 吴永宁[1] 

机构地区：[1]国家食品安全风险评估中心,卫生部食品安全风险评估重点实验室,北京100021

出　　处：《食品安全质量检测学报》2014年第2期468-474,共7页Journal of Food Safety and Quality

摘　　要：目的通过优化程序升温蒸发进样口的相关参数,建立测定食品中多氯代二苯并二噁英和多氯代二苯并呋喃(PCDD/Fs)的程序升温大体积进样高分辨气相色谱-高分辨质谱(HRGC-HRMS)方法。方法食品样品提取、净化分离和浓缩按《GB/T 5009.205-2007食品中二噁英及其类似物毒性当量的测定》规定进行,待测试样进样15μL,应用HRGC-HRMS结合同位素稀释技术测定其中PCDD/Fs。结果最佳条件为进样口初始温度115℃,蒸发相温度140℃,蒸发相吹扫流速为5 mL。大体积进样所获得的待测物峰面积及S/N存在显著增加(P<0.05)。结论程序升温大体积进样方式能显著提高食品基质中PCDD/Fs的检测能力,有助于保证食品安全风险评估结果的准确可靠。Objective By optimizing critical parameters of programmable temperature vaporizer (PTV), a method of PTV-based large volume injection was established for the determination of PCDD/Fs in various food samples using HRGC-HRMS. Methods The preparation of food, including extraction, clean-up, separation and concentration, was carried out depending on GB/T5009.205-2007 “Determination of Toxic Equivalencies of Dioxin and Dioxin-like Compounds in Foods”. The injection volume of extracts was 15μL, and the analyte was subsequently determined by using HRGC-HRMS with isotopic dilution. Results The optimized parame-ter of the initial temperature of PTV injector, the temperature of evaporation phase, and the flow rate of evapo-ration phase was set at 115℃, 140℃, and 5 mL/min, respectively. Peak area and the ratio of signal to noise (S/N) of PCDD/F congeners significantly increased using PTV-based large volume injection (P<0.05). Conclu-sion The method of PTV-based large volume injection can notably raise the competence of determining PCDD/Fs in food, which may help to assess the food safety risk more accurately and reliably.

关 键 词：程序升温蒸发 大体积进样 噁多氯代二苯并二 英和多氯代二苯并呋喃 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]