液相色谱串联质谱法同时测定凡纳滨对虾中的27种抗寄生虫药物残留

Determination of 27 antiparasitic drug residues in Penaeus vannamei by liquid chromatography-tandem mass spectrometry simultaneously

目的:规范凡纳滨对虾抗寄生虫药物的使用。方法:用80%乙腈水溶液提取凡纳滨对虾样品中的抗寄生虫药物,经C 18和中性氧化铝粉净化后,超高效液相色谱—串联质谱分析。药物经Thermo Hypersil Gold aQ色谱柱分离,0.1%甲酸—乙腈和10 mmol/L甲酸铵溶液(含0.1%甲酸)分别作为有机相和水相进行梯度洗脱,采用电喷雾离子源正负离子同步扫描,多反应监测模式,基质匹配标准溶液外标法定量分析。结果:27种抗寄生虫药物在一定浓度范围内皮尔森相关系数(r)大于0.9741,线性关系良好;检出限为0.5~2.0μg/kg,定量限为2~5μg/kg;空白样品在5,10,50μg/kg 3个添加水平下的方法加标回收率(n=6)为61.90%~118.54%,批内变异系数(n=6)为0.57%~12.56%,批间变异系数(n=3)为1.29%~16.47%。结论:该方法选择性好,回收率、精密度高,测定周期短,可满足实验室的检测需要。

Objective:An ultra-high performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of 27 antiparasitic drug residues in Litopenaeus vannamei.Methods:The solution was used to extract antiparasitic drugs in the samples of L.vannamei.The supernatant after centrifugation was purified by C 18 and neutral alumina powder.The sample solution was analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry and applied to the instrument workstation to perform data analysis.A Thermo Hypersil Gold aQ column was used as the separation column,and 0.1%formic acid acetonitrile and 10 mmol/L ammonium formate solution(containing 0.1%formic acid)were invoked as the organic phase and the aqueous phase for gradient elution,respectively.The electrospray ion source was used for positive and negative ion synchronous scanning and multiple reaction monitoring modes.The ion abundance ratio was qualitative,and the matrix-matched reference solution external standard method was employed for quantitative analysis.The results showed that the Pearson correlation coefficient(r)of 27 antiparasitic drugs was greater than 0.9741 in a certain concentration range,and the linear relationship was good.Results:The detection limit was 0.5~2.0μg/kg,and the quantification limit was 2~5μg/kg;The recoveries(n=6)of the method spiked at the low,medium and high concentration levels of the samples were 61.90%~118.54%,the intra-assay coefficient of variation(n=6)was 0.57%~12.56%,and the inter-assay coefficient of variation(n=3)was 1.29%~16.47%.Conclusion:The method has good selectivity,high method recovery rate,high precision,and short measurement period,provides a robust and efficient method for the determination of antiparasitic drugs in the laboratory,and meets the testing needs of the laboratory.