Choi Jeong-Min, Zheng Weijia, Abd El-Aty A M, Kim Seong-Kwan, Park Da-Hee, Yoo Kyung-Hee, Lee Gyu-Hee, Baranenko Denis A, Hacımüftüoğlu Ahmet, Jeong Ji Hoon, Kang Young-Sun, Shin Ho-Chul
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.
Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, Giza, Egypt.
Biomed Chromatogr. 2019 Jul;33(7):e4522. doi: 10.1002/bmc.4522. Epub 2019 Apr 7.
We developed an analytical method using liquid-liquid extraction (LLE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) to detect and quantify tebufenozide (TEB) and indoxacarb (IND) residues in animal and aquatic products (chicken muscle, milk, egg, eel, flatfish, and shrimp). The target compounds were extracted using 1% acetic acid (0.1% acetic acid for egg only) in acetonitrile and purified using n-hexane. The analytes were separated on a Gemini-NX C column using (a) distilled water with 0.1% formic acid and 5 mm ammonium acetate and (b) methanol with 0.1% formic acid as the mobile phase. All six-point matrix-matched calibration curves showed good linearity with coefficients of determination (R ) ≥0.9864 over a concentration range of 5-50 μg/kg. Intra- and inter-day accuracy was expressed as the recovery rate at three spiking levels and ranged between 73.22 and 114.93% in all matrices, with a relative standard deviation (RSD, corresponding to precision) ≤13.87%. The limits of quantification (LOQ) of all target analytes ranged from 2 to 20 μg/kg, which were substantially lower than the maximum residue limits (MRLs) specified by the regulatory agencies of different countries. All samples were collected from different markets in Seoul, Republic of Korea, and tested negative for tebufenozide and indoxacarb residues. These results show that the method developed is robust and may be a promising tool to detect trace levels of the target analytes in animal products.
我们开发了一种采用液液萃取(LLE)和液相色谱 - 串联质谱(LC-MS/MS)的分析方法,用于检测和定量动物及水产品(鸡肉、牛奶、鸡蛋、鳗鱼、比目鱼和虾)中的虫酰肼(TEB)和茚虫威(IND)残留。目标化合物用乙腈中的1%乙酸(仅鸡蛋用0.1%乙酸)萃取,并用正己烷纯化。分析物在Gemini-NX C柱上分离,流动相为:(a)含0.1%甲酸和5 mM乙酸铵的蒸馏水,(b)含0.1%甲酸的甲醇。所有六点基质匹配校准曲线在5 - 50 μg/kg浓度范围内显示出良好的线性,决定系数(R²)≥0.9864。日内和日间准确度以三个加标水平下的回收率表示,所有基质中的回收率在73.22%至114.93%之间,相对标准偏差(RSD,对应精密度)≤13.87%。所有目标分析物的定量限(LOQ)范围为2至20 μg/kg,远低于不同国家监管机构规定的最大残留限量(MRLs)。所有样品均采集自韩国首尔的不同市场,虫酰肼和茚虫威残留检测均为阴性。这些结果表明,所开发的方法稳健,可能是检测动物产品中痕量目标分析物的一种有前景的工具。