通过衍生化-气相色谱串联质谱法对鸡蛋中癸氧喹酯残留量进行定量分析
Quantitative Analysis of Decoquinate Residues in Hen Eggs through Derivatization-Gas Chromatography Tandem Mass Spectrometry.
作者信息
Zhu Yali, Chen Lan, Guo Yawen, Gao Pengfei, Liu Shuyu, Zhang Tao, Zhang Genxi, Xie Kaizhou
机构信息
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China.
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China.
出版信息
Foods. 2023 Dec 29;13(1):119. doi: 10.3390/foods13010119.
A novel precolumn derivatization-gas chromatography tandem mass spectrometry (GC-MS/MS) method was developed to detect and confirm the presence of decoquinate residues in eggs (whole egg, albumen and yolk). Liquid-liquid extraction (LLE) and solid phase extraction (SPE) were used to extract and purify samples. The derivatization reagents were pyridine and acetic anhydride, and the derivatives were subjected to GC-MS/MS detection. After the experimental conditions were optimized, satisfactory sensitivity was obtained. The limits of detection (LODs) and limits of quantification (LOQs) for the decoquinate in eggs (whole egg, albumen and yolk) were 1.4-2.4 μg/kg and 2.1-4.9 μg/kg, respectively. At four spiked concentration levels, the average recoveries were 74.3-89.8%, the intraday RSDs ranged from 1.22% to 4.78%, and the inter-day RSDs ranged from 1.61% to 7.54%. The feasibility and practicality of the method were confirmed by testing egg samples from a local supermarket.
建立了一种新型的柱前衍生化-气相色谱串联质谱（GC-MS/MS）方法，用于检测和确证鸡蛋（全蛋、蛋清和蛋黄）中地克珠利残留量。采用液液萃取（LLE）和固相萃取（SPE）对样品进行提取和净化。衍生化试剂为吡啶和乙酸酐，衍生物进行GC-MS/MS检测。优化实验条件后，获得了满意的灵敏度。鸡蛋（全蛋、蛋清和蛋黄）中地克珠利的检测限（LOD）和定量限（LOQ）分别为1.4 - 2.4 μg/kg和2.1 - 4.9 μg/kg。在四个加标浓度水平下，平均回收率为74.3% - 89.8%，日内相对标准偏差（RSD）为1.22%至4.78%，日间RSD为1.61%至7.54%。通过检测当地超市的鸡蛋样品，证实了该方法的可行性和实用性。
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