1.Agricultural Products Quality Safety Center of Changzhou;2.College of Environmental Science and Engineering,Changzhou University
Detection and source analysis of diazepam residues in aquaculture from Changzhou
本文分析水产养殖中饲料、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0.5～20μg/L 范围内线性良好，相关系数（r2）均大于0.999；在饵料、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；三种基质中1.0μg/kg、5.0μg/kg和10.0μg/kg三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%，浓度范围为2.2~213090μg/kg；10份诱鱼剂中均检出DZP检出率达100%，浓度范围为637~3471mg/kg；27份水样中DZP检出率达85.2%，浓度范围为0.4~9.8μg/L和71份淡水鱼中DZP的检出率为54.9%，浓度范围为0.5~21.8μg/ kg。由此可见窝料、饵料及诱鱼剂的使用可能是养殖水体和水产品中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 content of Diazepam(DZP) in feed, nest material, fish bait, water samples and quatic products in aquaculture, and a quantitative detection method using online purification-liquid chromatography tandem mass spectrometry has been established. The results showed that the linearity of DZP content was good in the range of 0.5 to 20μg/L, the correlation coefficient (r2) was greater than 0.999, and the LOQs of this method was 1.0μg/kg, 0.5μg/L, and 1.0μg/kg in fish bait ,water samples and aquatic products respectively. The average recoveries of DZP ranged from 85.2% to 106.5%, 82.3% to 108.0%, and 90.7% to 116.0% spiked at 1.0 μg/kg, 5.0 μg/kg and 10.0 μg/kg with the relative standard deviation (RSD) ranged from 3.6% to 5.1%, 2.7% to 4.3%, 2.1% to 2.6%, respectively. The results showed that DZP was not detected in 7samples of feed for aquaculture,the detection rate of DZP in 28 samples of the nest material and fish bait used in fishing reached 66.7%, with a concentration range from 2.2 to 213090 μg/kg , the detection rate of DZP in 10 samples of the fish attractants reached 100%, with a concentration range from 637 to 3471mg/kg, the detection rate of DZP in 27 water samples was 85.2% , with a concentration range from 0.4 to 9.8μg/L and the detection rate of DZP in 71 fish samples was 54.9%, with a concentration range from 0.5 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 diazepam in aquaculture water environment and aquatic products, which poses potential risks to consumer food safety and the healthy development of the aquaculture industry. It is strengthen the supervision and monitoring of DZP.