超高效液相色谱-串联质谱法测定添加剂预混合饲料中3种异噻唑啉酮杀菌剂的研究

Determination of three isothiazolinone fungicides in additive premixed feed by ultra-high performance liquid chromatography tandem mass spectrometry

试验旨在建立添加剂预混合饲料中3种噻唑啉酮类药物的超高效液相色谱-串联质谱测定方法(UPLC-MS/MS)。饲料样品经乙腈提取后,使用Prime HLB小柱净化,以SB-C18(100 mm×3 mm,1.8μm)作为分析柱,甲醇和水作为流动相进行梯度洗脱。在电喷雾正离子模式下,进行检测;使用基质匹配外标法测定3种异噻唑啉酮类药物的含量,并对所建方法的线性关系、检出限、定量限、回收率、准确度、精密度等指标进行考察。结果显示,在0.25~500.00μg/L范围内线性关系良好,3种目标物的相关系数(R^(2))均大于0.9900;检出限、定量限分别为10μg/kg和30μg/kg。3种异噻唑啉酮类药物的回收率在69.8%~99.9%之间,相对标准偏差(RSD)在4.2%~10.0%之间。研究表明,试验所用方法操作简单、灵敏度高且定量准确,适用于测定添加剂预混合饲料中3种异噻唑啉酮类药物含量,可为养殖环节投入品中异噻唑啉酮类药物污染筛查提供准确高效的技术手段,从源头保障动物源性产品安全。

The experiment aims to establish an ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the determination of three isothiazolinone drugs in additive premixed feed.After extracting feed samples with acetonitrile,they were purified using Prime HLB columns and treated with SB-C18(100 mm×3.0 mm,1.8μm).As an analytical column,methanol and water are used as mobile phases for gradient elution.In the positive ion mode of electric spray,the detection is carried out.Use matrix matching external standard method to determine the content of three isothiazolinone drugs,and examine the linear relationship,detection limit,quantification limit,recovery rate,accuracy,precision,and other indicators of the established method.The results showed a good linear relationship within the range of 0.25~500.00μg/L,with correlation coefficients(R^(2))>0.9900.The detection limit is 10μg/kg,quantification limit of 30μg/kg.The recovery rates of the three isothiazolone drugs range from 69.8%to 99.9%,with relative standard deviations(RSD)ranging from 4.2%to 10.0%.Research has shown that the method used in the experiment is simple to operate,highly sensitive,and quantitatively accurate.It is suitable for measuring the content of three isothiazolidone drugs in additive premixed feed.It can provide an accurate and efficient technical means for screening the contamination of three isothiazolidone drugs in input products in the breeding process,and ensure the safety of animal-derived products from the source.