超高效液相色谱-串联质谱法同时测定水产品中三苯甲烷类染料和氯霉素类药物的残留量  

Simultaneous determination of triphenylmethane dyes and Chloramphenicols residues in aquatic products by ultra performance liquid chromatography tandem mass spectrometry

作　　者：万承波 万建春 罗秋红 占春瑞 WAN Chengbo;WAN Jianchun;LUO Qiuhong;ZHAN Chunrui(Jiangxi Provincial Produce Quality Supervision Testing Institute,Nanchang 330052,China;Technology Center of Nanchang Customs District,Nanchang 330038,China)

机构地区：[1]江西省产品质量监督检测院,江西南昌330052 [2]南昌海关技术中心,江西南昌330038

出　　处：《南昌大学学报（理科版）》2020年第6期579-584,592,共7页Journal of Nanchang University(Natural Science)

摘　　要：建立了超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定水产品中三苯甲烷染料和氯霉素类药物。样品用乙腈均质提取,中性氧化铝净化,氮吹至干后,乙酸铵乙腈溶液(1+1,v:v)定容,质谱仪分别在正负模式测定,内标法定量。三苯甲烷染料定量限为0.5μg·kg^(-1),氯霉素定量限为0.1μg·kg^(-1),甲砜霉素和氟甲砜霉素定量限为1.0μg·kg^(-1)。三苯甲烷染料在0.25~5.0μg·kg^(-1),氯霉素在0.05~2.0μg·kg^(-1),甲砜霉素和氟甲砜霉素在0.5~20.0μg·kg^(-1)浓度范围内,线性相关系数均在0.99以上。鳗鱼、小龙虾和鲤鱼样品添加7种化合物,在1、2和4倍定量限浓度水平回收率在61.5~119.0%范围内,RSD值在0.76~14.46%之间。方法改进了氯霉素类药物残留检测前处理方法,实现了水产品中三苯甲烷类染料和氯霉素类药物残留量同时检测,可为实际检测提供高效、准确、可靠的解决方案。An ultra performance liquid chromatography tandem mass spectrometry method was developed for the determination of triphenylmethane dyes and Chloramphenicols in aquatic products.The samples were extracted with acetonitrile and purified by neutral alumina.After nitrogen blowing to dryness,the constant volume was with ammonium acetate acetonitrile solution(1+1,V:V).The limit of quantification was 0.5μg·kg^(-1) in triphenylmethane dye,the limit of quantification was 0.1μg·kg^(-1) in chloramphenicol,and the limit of quantification was 1.0μg·kg^(-1) in thiamphenicol and florfenicol.The linear correlation coefficients were above 0.99 in the concentration range of 0.25~5.0μg·kg^(-1) for triphenylmethane,0.05~2.0μg·kg^(-1) for chloramphenicol,and 0.5~20.0μg·kg^(-1) for thiamphenicol and florfenicol.The recoveries of eels,crayfish and carp samples were in the range of 61.5-119.0%with RSD of 0.76~14.46%at 1,2 and 4-fold limit of quantitation levels.The pretreatment method of chloramphenicol residues detection was improved.The simultaneous detection of triphenylmethane dyes and chloramphenicol residues in aquatic products was realized,and it could provide an efficient,accurate and reliable solution for the actual detection.

关 键 词：UHPLC-MS/MS 水产品 三苯甲烷染料 氯霉素类 

分 类 号：TS201.6[轻工技术与工程—食品科学]