Institute of Quality Standards and Testing Technology for Agricultural Products, Chinese Academy of Agricultural Science, Beijing 100081, China.
Institute of Quality Standards and Testing Technology for Agricultural Products, Chinese Academy of Agricultural Science, Beijing 100081, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Sep 15;1095:183-190. doi: 10.1016/j.jchromb.2018.07.025. Epub 2018 Jul 21.
In this study, a method for simultaneous determination of 40 antibiotics from 6 different drug families (7 quinolones, 5 penicillins, 8 macrolides, 2 lincosamides, 4 tetracyclines, and 13 sulfonamides) and 3 amantadines in animal-derived feedstuffs (ADF) through ultraperformance liquid chromatography-tandem mass spectrometry using a new lipid-removing solid-phase extraction column PRiME HLB was developed. The sample was extracted with 20 mL extraction solution and then purified and concentrated with PRiME HLB. The eluent was evaporated to dryness under nitrogen and analyzed with LC-MS/MS using acetonitrile and 0.1% formic acid as the mobile phase via gradient elution. Under the optimum conditions, recoveries were 65.8% to 104.4% with a relative standard deviation of <15% at spiked levels of 5.0 μg/kg to 100 μg/kg. The limits of detection ranged from 0.5 μg/kg to 5 μg/kg. 15 of the 43 drugs were found in ADF. Sulfonamides, fluoroquinolones, macrolides, tetracyclines, and amantadines were detected, with the highest levels reaching 325 μg/kg.
本研究建立了一种利用新型去脂固相萃取柱 PRiME HLB 通过超高效液相色谱-串联质谱法同时检测动物源性饲料（ADF）中 6 种不同药物家族（7 种喹诺酮类、5 种青霉素类、8 种大环内酯类、2 种林可酰胺类、4 种四环素类和 13 种磺胺类）和 3 种金刚烷胺类 40 种抗生素的方法。采用 20 mL 提取溶液提取样品，然后用 PRiME HLB 进行纯化和浓缩。洗脱液在氮气下蒸发至干，用乙腈和 0.1%甲酸作为流动相，通过梯度洗脱，用 LC-MS/MS 进行分析。在最佳条件下，5.0μg/kg 至 100μg/kg 加标水平下，回收率为 65.8%至 104.4%，相对标准偏差<15%。检测限范围为 0.5μg/kg 至 5μg/kg。在 ADF 中发现了 15 种 43 种药物。检测到磺胺类、氟喹诺酮类、大环内酯类、四环素类和金刚烷胺类，最高水平达到 325μg/kg。
