Ministry of Agriculture, Livestock and Food Supply (MAPA), Agricultural National Laboratory, Lanagro/MG, Brazil.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(4):517-25. doi: 10.1080/19440049.2011.623681. Epub 2011 Nov 8.
The use of aminoglycoside antibiotics in food animals is approved in Brazil. Accordingly, Brazilian food safety legislation sets maximum levels for these drugs in tissues from these animals in an effort to guarantee that food safety is not compromised. Aiming to monitor the levels of these drugs in tissues from food animals, the validation of a quantitative, confirmatory method for the detection of residues of 10 aminoglycosides antibiotics in poultry, swine, equine and bovine kidney, with extraction using a solid phase and detection and quantification by LC-MS/MS was performed. The procedure is an adaptation of the US Department of Agriculture, Food Safety and Inspection Service (USDA-FSIS) qualitative method, with the inclusion of additional clean-up and quantification at lower levels, which proved more efficient. Extraction was performed using a phosphate buffer containing trifluoroacetic acid followed by neutralization, purification on a cationic exchange SPE cartridge, with elution with methanol/acetic acid, evaporation, and dilution in ion-pair solvent. The method was validated according to the criteria and requirements of the European Commission Decision 2002/657/EC, showing selectivity with no matrix interference. Linearity was established for all analytes using the method of weighted minimum squares. CCα and CCβ varied between 1036 and 12,293 µg kg(-1), and between 1073 and 14,588 µg kg(-1), respectively. The limits of quantification varied between 27 and 688 µg kg(-1). The values of recovery for all analytes in poultry kidney, fortified in the range of 500-1500 µg kg(-1), were higher than 90%, and the relative standard deviations were lower than 15%, except spectinomycin (21.8%). Uncertainty was estimated using a simplified methodology of 'bottom-up' and 'top-down' strategies. The results showed that this method is effective for the quantification and confirmation of aminoglycoside residues and could be used by the Brazilian programme of residue control.
巴西批准在食用动物中使用氨基糖苷类抗生素。因此，巴西食品安全法规为这些动物组织中的这些药物设定了最大残留限量，以确保食品安全不受影响。为了监测食用动物组织中这些药物的水平，对一种定量、确证方法进行了验证，用于检测和定量检测家禽、猪、马和牛肾组织中 10 种氨基糖苷类抗生素的残留，采用固相提取，LC-MS/MS 检测。该程序是美国农业部食品安全检验局（USDA-FSIS）定性方法的改编，包括在较低水平进行额外的净化和定量，这被证明更有效。提取采用含三氟乙酸的磷酸盐缓冲液进行，然后进行中和，在阳离子交换 SPE 柱上进行净化，用甲醇/乙酸洗脱，蒸发，并用离子对溶剂稀释。该方法根据欧盟委员会第 2002/657/EC 号决定的标准和要求进行了验证，显示出无基质干扰的选择性。使用加权最小二乘法对所有分析物建立了线性关系。CCα和 CCβ分别在 1036 和 12293 µg kg(-1) 之间和 1073 和 14588 µg kg(-1) 之间变化。定量限在 27 和 688 µg kg(-1) 之间变化。在鸡肾中，所有分析物的回收率均高于 90%，相对标准偏差均低于 15%，除壮观霉素（21.8%）外，回收率在 500-1500 µg kg(-1) 范围内添加。使用“自下而上”和“自上而下”策略的简化方法估计了不确定性。结果表明，该方法对氨基糖苷类残留的定量和确证有效，可用于巴西残留控制计划。
