通过混合模式吸附剂净化，建立了高效液相色谱串联四极杆/静电场轨道离子阱高分辨率质谱法（Q Exactive HF，HRMS）同步测定鸡蛋中磺胺喹噁啉和二甲氧苄啶的分析方法。鸡蛋样品经过溶剂超声提取，提取液8000 r/min高速离心后，通过添加多重机制杂质吸附净化填料净化并收集，40 ℃氮气吹干，用0.1%甲酸-乙腈溶液（9:1，V/V）定容进行质谱分析。采用Acquity UPLC BEH C18（2.1 mm×100 mm，1.7 μm）色谱柱进行分离，以0.1%甲酸水和0.1%甲酸甲醇作为流动相，进行梯度洗脱。质谱采用平行反应监测扫描模式实现对目标化合物的定量分析。在所建立的色谱条件下，2种化合物能够得到较好的分离，在线性范围内线性关系良好，相关系数均大于0.999。通过加标验证，在10、50、200 ng/g加标水平下，2种化合物平均回收率为96.4%~106.8%，相对标准偏差（RSD）小于7.1%。方法检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.1~0.2 μg/kg和0.3~0.6 μg/kg。本方法样品处理过程简便、分析时间短，准确可靠、灵敏度高，适用于鸡蛋中磺胺喹噁啉及增效剂的同步测定。

A high-performance liquid chromatography-tandem quadrupole electrostatic-ion-trap high-resolution mass spectrometry (Q Exactive HF, HRMS) method with mixed-mode-adsorbent-based purification was established for the simultaneous determination of sulfaquinoxaline and diaveridine in eggs. The egg samples were first extracted by ultrasonic solvent extraction, followed by centrifugation of the extracts at 8000 r/min, and purification and collection via the addition of adsorbents with different operating mechanisms. The extracts were subsequently dried under nitrogen at 40 ℃, followed by the addition of 0.1% formic acid-acetonitrile solution (9:1, V/V) to prepare constant-volume samples suitable for mass spectrometry. An Acquity ultra-performance liquid chromatography (UPLC) Beh C18 (2.1 mm×100 mm, 1.7 μm) column was employed for separation, with 0.1% formic acid-water and 0.1% formic acid-methanol being used as the mobile phases for gradient elution. Mass spectrometry was conducted in the parallel reaction monitoring mode for the quantitative analysis of the target compounds. The two investigated compounds could be adequately separated under the established chromatographic conditions. Acceptable linear relationships in the linear range, and correlation coefficients greater than 0.999 were obtained. Standard addition validation at addition levels of 10, 50, and 200 ng/g resulted in average recoveries of 96.4%~106.8% of the two compounds being obtained, with relative standard deviations (RSDs) of less than 7.1%. The limit of detection (LOD, S/N=3) and limit of quantification (LOQ, S/N=10) of the developed method were found to be 0.1~0.2 μg/kg and 0.3~0.6 μg/kg, respectively. This method requires straightforward sample processing and enables a short duration of analysis, while ensuring accuracy, reliability, and high sensitivity, thereby establishing its suitability for the simultaneous determination of sulfaquinoxaline and sulfonamide potentiators in eggs.

国家重点研发计划项目（2018YFC1602302）；国家自然科学基金资助项目（31572443）