色谱-质谱法鉴定鱼饵窝料及鱼样中地西泮的方法研究  

Identification and analysis of diazepam in fish bait nest material and fish samples by chromatography-mass spectrometry

作　　者：方咏霓 徐国华 储兰 裴克梅[1] 赵蒙 褚建新 王朝虹 吕凌 毛闽燕 董银利 Fang Yongni;Xu Guohua;Chu Lan;Pei Kemei;Zhao Meng;Chu Jianxin;Wang Zhaohong;Lv Ling;Mao Minyan;Dong Yinli(School of Chemistry and Chemical Engineering,Zhejiang Sci-Tech University,Hangzhou,Zhejiang 310018;Zhejiang Ecological Environment Science Design and Research Institute,Hangzhou,Zhejiang 310013;Procuratoral Technology and Information Research Center,Supreme People’s Procuratorate,Beijing 100144;The People's Procuratorate of Zhejiang province,Hangzhou,Zhejiang 310013;The People's Procuratorate of wenzhou,Wenzou,Zhejiang 325014;The People's Procuratorate of Jiangshan,Jiangshan,Zhejiang 324100;Judicial Identification Center of Xinjiang Police College,Xinjiang Urumqi 830000)

机构地区：[1]浙江理工大学化学与化工学院,浙江杭州310018 [2]浙江省生态环境科学设计研究院,浙江杭州310013 [3]最高人民检察院检察技术信息研究中心,北京100144 [4]浙江省人民检察院,浙江杭州310013 [5]温州市人民检察院,浙江温州325014 [6]江山市人民检察院,浙江江山324100 [7]新疆警察学院司法鉴定中心,新疆乌鲁木齐830000

出　　处：《中国法医学杂志》2024年第5期585-589,595,共6页Chinese Journal of Forensic Medicine

摘　　要：目的 建立将气相色谱-串联质谱法(GC-MS)和液相色谱-串联质谱法(LC-MS)相结合的分析方法,检测鱼饵窝料、鱼样中地西泮的残留量,并改进样品的预处理步骤,使得实验结果准确、样品处理方便快捷。方法以地西泮为研究对象,样品根据类型分别使用甲醇和二氯甲烷/正己烷作为溶剂进行萃取,离心后取上清液上机检测。结果 地西泮标样在10~10 000 ng/mL范围内呈现良好的线性关系,在甲醇和混合溶剂中的保留时间分别为13.54 min和13.83 min,相关系数分别为0.998和0.999;使用甲醇萃取溶剂的检测限为2 ppb,定量限为6 ppb。使用混合溶剂的检测限为5 ppb,定量限为15 ppb;当样品为鱼饵窝料时,GC-MS谱图清晰标准,峰形尖锐突出;当样品为生物检材时,GC-MS谱图受基质干扰严重,而LC-MS数据更为准确快捷。结论 鱼饵窝料使用GC-MS测定含量更为合适,鱼样由于生物体的复杂性,使用LC-MS测定含量更准确。Objective To establish an analytical method combining gas chromatography-tandem mass spectrometry(GCMS)and liquid chromatography-tandem mass spectrometry(LC-MS)to detect diazepam residue in bait nest materials and fish samples,and improve the pretreatment steps of samples to make the experimental results accurate and the sample processing convenient and fast.Methods Taking diazepam as the research object,samples were extracted with methanol and dichloromethane/n-hexane as solvents according to the type,and the supernatant was taken for detection after centrifugation.Results The diazepam standard sample showed a good linear relationship in the range of 10~10000 ng/mL.The retention times in methanol and mixed solvent were 13.54 min and 13.83 min,respectively,and the correlation coefficients were 0.998 and 0.999,respectively;The limit of detection(LOD)of using methanol as extraction solvent was 2 ppb,and limit of quantification(LOQ)was 6 ppb.The LOD of using mixed solvents was 5 ppb,and the LOQ was 15 ppb.When the sample is a bait nest material,the GC-MS spectrum was clear and standard,and the peak shape was sharp and prominent;When the sample is biological specimen,the GC-MS spectra are disturbed by matrix,while the LC-MS data is more accurate and faster.Conclusion It is more appropriate to use GC-MS to determine the content of bait nest materialsamples,and it is more accurate to LC-MS to determine the content of fish samples due to the complexity of the organism.

关 键 词：液相色谱-串联质谱 气相色谱-串联质谱 地西泮 生物检材 水产品 

分 类 号：D918.93[政治法律—法学]