常州地区水产养殖中地西泮残留检测及来源分析

Determination and source analysis of diazepam residues in aquaculture in Changzhou area

本研究分析了水产养殖和垂钓中饲料、窝料、饵料、水样及水产品中地西泮(Diazepam,DZP)的存在情况,并建立了在线净化-液相色谱串联质谱定量检测方法。结果表明DZP含量在0.5~20.0μg/L间线性良好,相关系数(r^(2))均大于0.999;饵料、水样和水产品中定量限(Limit of quantitation,LOQ)分别为1.0μg/kg、0.5μg/L、1.0μg/kg;3种基质中1.0μg/kg、5.0μg/kg和10.0μg/kg 3个浓度水平的加标回收率分别为85.2%~106.5%、82.3%~108.0%、90.7%~116.0%,相对标准偏差(Relative standard deviation,RSD)分别为3.6%~5.1%、2.7%~4.3%、2.1%~2.6%。通过调查发现,7份养殖用饲料中均未检出DZP;28份垂钓中使用的窝料、饵料检出率达66.7%,浓度为2.2~213090.0μg/kg;10份诱鱼剂中均检出DZP,检出率达100%,浓度为637000.0~3471000.0μg/kg;27份水样中DZP检出率达85.2%,浓度为0.4~9.8μg/L和71份淡水鱼中DZP的检出率为54.9%,浓度为0.5~21.8μg/kg。由此可见窝料、饵料及诱鱼剂的使用可能是水体和水产品中DZP频繁检出的重要原因之一,对消费者食用安全和水产养殖行业的健康发展均具有潜在风险,亟需加强DZP监管和监测。

This study investigated the presence of Diazepam(DZP)in feed,nest material,fish bait,water samples,and aquatic products in aquaculture,and a quantitative detection method was developed using online purification-liquid chromatography-tandem mass spectrometry.Results showed that the DZP content exhibited good linearity in the range of 0.5 to 20.0μg/L,with a correlation coefficient(r^(2))exceeding 0.999.The limit of quantification(LOQ)for this method was determined to be 1.0μg/kg for fish bait,0.5μg/L for water samples,and 1.0μg/kg for aquatic products.The average recoveries of DZP ranged from 85.2%to 106.5%,82.3%to 108.0%,and 90.7%to 116.0%at spike-in levels of 1.0μg/kg,5.0μg/kg and 10.0μg/kg,with relative standard deviation(RSD)falling within 3.6%to 5.1%,2.7%to 4.3%,and 2.1%to 2.6%,respectively.The findings revealed that DZP was not detected in 7 feed samples for aquaculture.However,the detection rate of DZP in 28 samples of nest material and fish bait used in fishing was 66.7%,with concentrations ranging from 2.2μg/kg to 213090.0μg/kg,Moreover,the detection rate of DZP in 10 samples of the fish attractants was 100%,with concentrations ranging from 637000.0μg/kg to 3471000.0μg/kg.Furthermore,27 water samples were found to have a detection rate of 85.2%,with concentrations ranging from 0.4μg/kg to 9.8μg/L.Lastly,the detection rate of DZP in 71 fish samples was 54.9%,with concentrations ranging from 0.5μg/kg to 21.8μg/kg.The use of nest material,fish bait,and fish attractants may be one of the important reasons for the frequent detection of DZP in aquaculture water environments and aquatic products,which could potentially pose risks to consumer food safety and the healthy development of the aquaculture industry.It is crucial to strengthen the supervision and monitoring of DZP.