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HLB-MCX-Based Solid-Phase Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry for the Simultaneous Determination of Four Agricultural Antibiotics (Kasugamycin, Validamycin A, Ningnanmycin, and Polyoxin B) Residues in Plant-Origin Foods

文献类型： 外文期刊

作者： Li, Wenxi 1 ; Dai, Xuefang 1 ; Pu, Entang 1 ; Bian, Haitao 2 ; Chen, Zilei 3 ; Zhang, Xueyan 1 ; Guo, Zhixiang 1 ; Li, Pe 1 ;

作者机构： 1.Yunnan Acad Agr Sci, Inst Agr Environm & Resource, Kunming 650205, Yunnan, Peoples R China

2.Dalian Ctr Certificat & Food & Drug Control, Dalian 116021, Peoples R China

3.Shandong Acad Agr Sci, Inst Qual Stand & Testing Technol Agroprod, Jinan 250100, Peoples R China

4.Shandong Prov Key Lab Testing Technol Food Qual &, Jinan 250100, Peoples R China

5.China Agr Univ, Coll Sci, Beijing 100193, Peoples R China

关键词： agricultural antibiotic pesticides; foods; SPE; HILIC; UPLC-MS/MS

期刊名称：JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY （ 影响因子：5.279； 五年影响因子：5.269 ）

ISSN： 0021-8561

年卷期： 2020 年 68 卷 47 期

页码：

收录情况： SCI

摘要： An ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of four highly polar agricultural antibiotics kasugamycin, validamycin A, ningnanmycin, and polyoxin B in plant-derived foods. The samples were extracted with a 0.2% formic acid solution, purified by hydrophilic-lipophilic balance and mixed-mode cation-exchange solid-phase extraction, and then reconstituted for UPLC-MS/MS detection. The chromatographic analysis was performed on a BEH Amide column (100 mm x 2.1 mm, 1.7 mu m) using gradient elution with a 0.1% formic acid solution and 0.1% formic acid acetonitrile as mobile phases. Method validation was performed on 15 matrices spiked at 0.02 (or 0.05), 0.5, and 2 mg/kg. The mean recovery rate ranged from 75 to 102% with relative standard deviations (RSD) was less than 20%. Good linearities (r > 0.99) in the range of 0.002-0.2 mu g/mL were obtained. The limits of quantification (LOQs) were 0.02 and 0.05 mg/kg. Studies on the stability of the analytes in the stored kiwifruit samples showed that kasugamycin, validamycin A, and ningnanmycin were stable for at least 6 months, while polyoxin B was observed to be partially degraded (the degradation rate at 6 months was 31.3%). The method was demonstrated to be effective and reliable in real samples. In the kiwifruit samples treated after 7 days, no residues of ningnanmycin and polyoxin B were detected, while the residues of kasugamycin and validamycin A were 0.12 and 0.038 mg/kg, respectively.

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