程序升温大体积进样在HRGC-HRMS法测定食品中PCDDF的应用
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15 μL, 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 15 μL, and the analyte was subsequently determined by using HRGC-HRMS with isotopic dilution. Results The optimized parameter of the initial temperature of PTV injector, the temperature of evaporation phase, and the flow rate of evaporation 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). Conclusion 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.
标题：程序升温大体积进样在HRGC-HRMS法测定食品中PCDDF的应用
英文标题：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 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
李敬光 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
赵云峰 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
吴永宁 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
中文关键词:程序升温蒸发,大体积进样,多氯代二苯并二噁英和多氯代二苯并呋喃。,
英文关键词:programmable temperature vaporization,large volume injection,PCDD/Fs,
发表日期：2013-11-15
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