CAJ | 학술논문

目的：通过优化程序升温蒸发进样口的相关参数,噁建立测定食品中多氯代二苯并二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噁食品中二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。
목적：통과우화정서승온증발진양구적상관삼수,오건립측정식품중다록대이분병이영화다록대이분병부남(PCDD/Fs)적정서승온대체적진양고분변기상색보-고분변질보(HRGC-HRMS)방법。방법식품양품제취、정화분리화농축안《GB/T 5009.205-2007오식품중이영급기유사물독성당량적측정》규정진행,대측시양진양15μL,응용HRGC-HRMS결합동위소희석기술측정기중PCDD/Fs。결과최가조건위진양구초시온도115℃,증발상온도140℃,증발상취소류속위5 mL。대체적진양소획득적대측물봉면적급S/N존재현저증가(P<0.05)。결론정서승온대체적진양방식능현저제고식품기질중PCDD/Fs적검측능력,유조우보증식품안전풍험평고결과적준학가고。
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.