Chen Rong, Chen Lan, Du Mingyue, Guo Qiaozhen, Zhong Ciping, Zhang Jing, Yu Xiaoqin
Key Laboratory of Liquor Regulation Technology, State Administration for Market Regulation, Sichuan Institute of Food Inspection, No. 8 Xinwen Road, West Hi-Tech Zone, Chengdu 611731, China.
Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention, Beijing 100013, China.
Foods. 2025 May 8;14(10):1660. doi: 10.3390/foods14101660.
A high-throughput method for the determination of a variety of chemical hazards in poultry muscle and egg samples was established via ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QqQ-MS). The sample preparation procedure was developed based on this quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and validated for 280 chemical hazards potentially present in poultry products. The target compounds in poultry samples were extracted with a 1% formic acid-acetonitrile solution (15:85, /), and the metal ions in the matrix were chelated by adding ethylenediaminetetraacetic acid disodium salt (NaEDTA). The supernatant was purified using Enhanced Matrix Removal (EMR) lipid sorbent. Chromatographic gradient separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with multiple reaction monitoring (MRM) under both negative- and positive-ion mode. Internal standard calibration or matrix-matched calibration was used for the quantitation. The results showed that good linearity was achieved for each target compound with correlation coefficients (R) ≥ 0.99. The limits of detection (LODs) ranged from 0.05 to 10 µg/kg, and the acceptable limits of quantification (LOQs) were determined to be 0.1-20 µg/kg for all 280 compounds. Approximately 90% of the target compounds exhibited mean recoveries ranging from 60% to 120%, with relative standard deviations (RSDs) within 16.2%. This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs due to its easy operation and high accuracy. It was applied in real sample detection, and 43 chemicals including metronidazole were found in 211 poultry samples, with a concentration range of 0.11-638 μg/kg.
通过超高效液相色谱-串联三重四极杆质谱法（UPLC-QqQ-MS）建立了一种用于测定家禽肌肉和蛋类样品中多种化学危害物的高通量方法。样品制备程序基于快速、简便、廉价、高效、耐用且安全（QuEChERS）的方法开发，并针对家禽产品中可能存在的280种化学危害物进行了验证。家禽样品中的目标化合物用1%甲酸-乙腈溶液（15:85，v/v）提取，基质中的金属离子通过添加乙二胺四乙酸二钠盐（NaEDTA）进行螯合。上清液使用增强型基质去除（EMR）脂质吸附剂进行净化。在ACQUITY UPLC BEH C18（2.1 mm×100 mm，1.7 μm）柱上进行色谱梯度分离，在负离子和正离子模式下均采用多反应监测（MRM）。定量采用内标校准或基质匹配校准。结果表明，各目标化合物均具有良好的线性，相关系数（R）≥0.99。所有280种化合物的检测限（LOD）范围为0.05至10 μg/kg，定量限（LOQ）为0.1 - 20 μg/kg。约90%的目标化合物平均回收率在60%至120%之间，相对标准偏差（RSD）在16.2%以内。该方法操作简便、准确性高，可用于禽蛋中违禁药物残留的高通量快速检测。将其应用于实际样品检测，在211份家禽样品中发现了包括甲硝唑在内的43种化学物质，浓度范围为0.11 - 638 μg/kg。
