Experiment Research Institute, National Agricultural Products Quality Management Service, 141, Yongjeon-ro, Gimcheon-si, Gyeongsangbuk-do 39660, Korea.
J Chromatogr A. 2023 Aug 30;1705:464170. doi: 10.1016/j.chroma.2023.464170. Epub 2023 Jun 22.
Extraction using acetonitrile and water and quadrupole time-of-flight mass spectrometry (LC and GC-QTOF/MS) techniques were used to screen for potential hazardous substances in livestock and pet hair. In addition, LC-MS/MS and GC-MS/MS techniques were used for verification of the analytical method and quantitative analysis of pesticides, veterinary drugs, mycotoxins and antioxidants in hair. Optimized sample preparation involves extracting 0.05 g of sample with 0.6 mL of ACN and 0.4 mL of distilled water. In addition, the two layers were separated by adding 0.1 g of NaCl. Then, both the ACN and water layers were analyzed by LC-TOF/MS, and the ACN layer was analyzed by GC-TOF/MS. Most of the matrix effects of livestock and pet hair were less than 50%, but some matrices and components showed high results, so matrix matching correction was applied for more precise quantification. Method validation was performed for 394 constituents (293 pesticides, 93 veterinary drugs, 6 mycotoxins and 2 preservatives) in dog, cat, cow and pig hair and chicken and duck feathers. All components showed good linearity (r2 ≥0.98) in the developed assay. The quantification limit of all compounds was set at 0.02 mg/kg, which is the lowest level that satisfies the recovery rate standard. The recovery experiment was repeated 8 times at 3 concentrations. Most of the components were extracted with the ACN layer, and the recovery rate was 63.35-119.98%. In order to confirm the efficiency of extracting harmful substances from actual samples, 30 hairs of livestock and pets were screened.
采用乙腈和水提取,并结合四极杆飞行时间质谱(LC 和 GC-QTOF/MS)技术,对畜产和宠物毛发中的潜在有害物质进行筛选。此外,还采用 LC-MS/MS 和 GC-MS/MS 技术对分析方法进行验证,并对毛发中的农药、兽药、真菌毒素和抗氧化剂进行定量分析。优化后的样品制备方法包括:用 0.6mL 乙腈和 0.4mL 蒸馏水提取 0.05g 样品,然后加入 0.1gNaCl 使两层分离。再分别用 LC-TOF/MS 分析乙腈层和水层,用 GC-TOF/MS 分析乙腈层。畜产和宠物毛发的大部分基质效应小于 50%,但有些基质和成分的基质效应较高,因此采用基质匹配校正进行更精确的定量。在狗、猫、牛和猪毛发以及鸡和鸭羽毛中对 394 种成分(293 种农药、93 种兽药、6 种真菌毒素和 2 种防腐剂)进行了方法验证。在开发的测定方法中,所有成分均呈现出良好的线性关系(r2≥0.98)。所有化合物的定量限均设定为 0.02mg/kg,这是满足回收率标准的最低水平。回收率实验在 3 个浓度下重复 8 次。大多数成分都用乙腈层提取,回收率为 63.35-119.98%。为了确认从实际样品中提取有害物质的效率,对 30 根畜产和宠物毛发进行了筛选。