College of Animal Science and Technology, Yangzhou University, Yangzhou, China.
Joint International Research Laboratory of Agriculture and Agri-Product Safety, Yangzhou University, Yangzhou, China.
Chirality. 2019 Oct;31(10):845-854. doi: 10.1002/chir.23117. Epub 2019 Aug 6.
Accelerated solvent extraction (ASE) and solid-phase extraction (SPE) conditions were optimized by a high-performance liquid chromatography-fluorescence detector (HPLC-FLD) method for the detection of piperazine in chicken tissues and pork. Piperazine residues were determined by precolumn derivatization with trimethylamine and dansyl chloride. Samples were extracted with 2% formic acid in acetonitrile using an ASE apparatus and purified using a Strata-X-C SPE column. The monosubstituted product of the reaction of piperazine with dansyl chloride was 1-dansyl piperazine (1-DNS-piperazine). Chromatographic separations were performed on an Athena C column (250 × 4.6 mm, id: 5 μm) with gradient elution using ultrapure water and acetonitrile (5:95, V/V) as the mobile phase. The calibration curves showed good linearity over a concentration range of LOQ-200.0 μg/kg with a coefficient of determination (R ) ≥ .9992. The recoveries and relative standard deviations (RSD values) ranged from 78.49% to 97.56% and 1.19% to 5.32%, respectively, across the limit of quantification (LOQ) and 0.5, 1, and 2.0 times the maximum residue limit (MRL; μg/kg). The limits of detection (LODs) and LOQs were 0.96 to 1.85 μg/kg and 3.20 to 5.50 μg/kg, respectively. The method was successfully applied for the validation of animal products in the laboratory.
加速溶剂萃取（ASE）和固相萃取（SPE）条件通过高效液相色谱-荧光检测器（HPLC-FLD）方法进行优化，用于检测鸡肉和猪肉中的哌嗪。哌嗪残留通过与三甲胺和丹磺酰氯的预柱衍生化来确定。样品用乙腈中的 2%甲酸通过 ASE 装置提取，并使用 Strata-X-C SPE 柱进行纯化。哌嗪与丹磺酰氯反应的单取代产物是 1-丹磺酰哌嗪（1-DNS-哌嗪）。在 Athena C 柱（250×4.6mm，id：5μm）上进行色谱分离，使用超纯水和乙腈（5：95，V/V）作为流动相进行梯度洗脱。校准曲线在 LOQ-200.0μg/kg 的浓度范围内表现出良好的线性，相关系数（R）≥.9992。回收率和相对标准偏差（RSD 值）的范围分别为 78.49%-97.56%和 1.19%-5.32%，跨越定量限（LOQ）和 0.5、1 和 2.0 倍最大残留限量（MRL；μg/kg）。检出限（LOD）和定量限（LOQ）分别为 0.96-1.85μg/kg 和 3.20-5.50μg/kg。该方法成功应用于实验室动物产品的验证。
