Identification and analysis of diazepam in fish bait nest material and fish samples by chromatography-mass spectrometry
10.13618/j.issn.1001-5728.2024.05.012
- VernacularTitle:色谱-质谱法鉴定鱼饵窝料及鱼样中地西泮的方法研究
- Author:
Yongni FANG
1
;
Guohua XU
;
Lan CHU
;
Kemei PEI
;
Meng ZHAO
;
Jianxin CHU
;
Zhaohong WANG
;
Ling LV
;
Minyan MAO
;
Yinli DONG
Author Information
1. 浙江理工大学化学与化工学院,浙江杭州 310018
- Keywords:
Liquid chromatography-tandem mass spectrometry;
Gas chromatography-tandem mass spectrometry;
Diazepam;
Biological samples;
Aquatic products
- From:
Chinese Journal of Forensic Medicine
2024;39(5):585-589,595
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish an analytical method combining gas chromatography-tandem mass spectrometry(GC-MS)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 10～10 000 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.
