脂质特异基质分散萃取超高效液相色谱-串联质谱法测定肉制品中4种兽药残留
胡雪郢,薛丰
重庆市渝中区疾病预防控制中心,重庆 400010
Determination of 4 agonist residues in meat by lipid-specific matrix dispersed purification combined with ultra performance liquid chromatography tandem mass spectrometry
胡雪郢,薛丰
The Yuzhong District Center for Disease Control and Prevention, Chongqing 400010, China
摘要:建立脂质特异性基质分散净化技术结合超高效液相色谱-串联质谱法检测肉制品中的4种β-受体激动剂类药物残留。向匀浆后的肉类样品中加入15 mL 0.2 mol/L的乙酸-乙酸钠缓冲溶液(pH 5.2)、100 μL β-葡萄糖醛酸苷肽酶/芳基磺酸脂酶和30 μL 1.0 μg/mL的含有4种目标化合物同位素标记的混合内标溶液,于(37±1)℃震荡酶解16.3 h,于4 ℃以12000 r/min离心10 min,取上清液分别经阳离子交换固相萃取和脂质特异性基质分散净化后,选择Welch Xtimate C18型色谱分离柱,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,样液经超高效液相色谱-串联质谱法测定,以同位素内标标准曲线法定量。4种β-受体激动剂的质量浓度在0.5~50 μg/L范围内线性良好,相关系数均大于0.997,检出限为0.1 μg/kg。以空白样品为基质进行加标回收试验,加标回收率为79.8%~95.6%,测定结果的相对标准偏差为2.47%~9.50%(n=6)。该方法适用于肉制品中4种β-受体激动剂类兽药残留的测定。
Abstract:A method for the determination of 4 agonist residues in meat was established by lipid-specific matrix dispersed purification combined with ultra performance liquid chromatography tandem mass spectrometry. The homogenized meat samples were added with 15 mL 0.2 mol/L sodium acetate buffer solution (pH 5.2), 100 μL β-glucuronidase and 30 μL 1.0 μg/mL mixed internal standard solution containing 4 isotopic labeling target compounds, shaked with enzyme hydrolysis at 37 ℃for 16.3 h, centrifuged at 12000 r/min for 10 min at 4 ℃. The supernatant was purified by mixed-mode, strong cation-exchange, reversed-phase, water-wettable polymer(MCX) and enhanced matrix removal(EMR)-Lipid QuEChERS respectively, and determined on a welch Xtimate C18 column by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) with a gradient elution program of methanol and 0.1% formic acid. The isotope internal standard curves were applied for the quantification. The mass concentration of 4 agonist residues had a good linear relationship with the chromatographic peak area in the range of ranges 0.5-50 μg/L with the correlation coefficient more than 0.997, and the detection limit was 0.1 μg/kg. The recovery rate was 79.8%-95.6%, and the relative standard deviation was 2.47%-9.50% (n=6). The method is suitable for the determination of 4 agonists in meat products.
关键词:脂质特性性基质分散萃取法;超高效液相色谱-串联质谱法;肉类; β-受体激动剂
Keywords:lipid-specific matrix dispersion; ultra performance liquid chromatography tandem mass spectrometry; meat; β-agonist
本文引用格式:
胡雪郢,薛丰.脂质特异基质分散萃取超高效液相色谱-串联质谱法测定肉制品中4种兽药残留[J].化学分析计量,2021,30(7):17.
Hu Xueying,Xue Feng. Determination of 4 agonist residues in meat by lipid-specific matrix dispersed purification combined with ultra performance liquid chromatography tandem mass spectrometry[J]. Chemical Analysis and Meterage,2021,30(7):17.
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