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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 To establish a procedure for the determination of polychlorinated dibenzodioxins and polychlorinated dibenzofurans (PCDD / Fs) in foods by optimizing the parameters of programmed temperature rising large-volume injection high-resolution gas chromatography- High-resolution mass spectrometry (HRGC-HRMS) method. Methods The extraction, purification, separation and concentration of food samples were carried out according to the provisions of GB / T 5009.205-2007 Determination of Toxicity of Dioxins and Analogues in Foodstuffs. The samples to be tested were injected 15μL. HRGC-HRMS combined with isotope dilution Among them, PCDD / Fs was measured. The optimum conditions were as follows: the initial inlet temperature was 115 ℃, the evaporation temperature was 140 ℃, and the purge flow rate was 5 mL. The peak area and S / N of the analyte obtained by large volume injection were significantly increased (P <0.05). Conclusion The large volume injection method of programmed temperature can significantly improve the detection ability of PCDD / Fs in food matrix and help to ensure the accuracy and reliability of food safety risk assessment.