Jingbo Zhang,Jing Hu,Shuai Wang,Xinping Lin,Huipeng Liang,Shengjie Li,Chenxu Yu,Xiuping Dong,Chaofan Ji
To effectively extract biogenic amines (BAs) from complex food matrices is an important issue. In this study, a stop-and-go-extraction tip (StageTip)-based method for simultaneous enrichment of six BAs including histamine, tyramine, putrescine, cadaverine, tryptamine, and β-phenylethylamine in fish samples was developed and optimized. This StageTip-based BAs extraction method required short extraction time, small sample size, and minimal consumption of organic solvents. In addition, an ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometer was used to identify and quantify BAs without derivatization. Target recovery efficiencies of BAs from spiked fish samples ranged from 84% to 110%. Linear regression models were established to determine BAs in the range of 0.4 to 3.0 mg/L ( R 2 > 0.995). Good repeatability was obtained with relative standard deviation of peak areas (1.17 to 5.61%) and retention time (0.09 to 0.20%). High sensitivity was achieved for the detection of six BAs (0.064 to 1.00 ng/L for the limit of detection, 0.10 to 5 ng/L for the limit of quantification). The proposed method had an obvious advantage in the analysis of BAs in complex food matrices such as fish tissues since it could reflect the subtle distribution of BAs from one fish fillet. Practical Application A StageTip-based BAs enrichment combined with UPLC-MS analysis method was developed and optimized, which was low - cost , environmentally friendly, and with good analytical performances. As such, it has the potential to become a powerful tool for the analysis of BAs in different complex food matrices.
Zhouhong Tan,Yunbo Wen,Kai Yang,Xia Zhao,Xiaoli Yang,Jieli He
The combined abuse of benzodiazepines and antipsychotics has become a global problem, and to develop a highly sensitive and selective method for monitoring of benzodiazepine hypnotics and antipsychotics is urgently necessary. In this work, we established a rapid method for the simultaneous determination of benzodiazepines (diazepam, alprazolam, triazolam, and estazolam) and antipsychotic drugs (clozapine, and chlorpromazine) based on ultra performance liquid chromatography-mass spectrometry (UPLC-MS). The accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), specificity, matrix effect and carry-over effect were verified in detail. The results of the recovery and repeat experiments proved that the proposed UPLC-MS method possessed very satisfactory accuracy and precision. The LOD and LOQ of the six psychoactive substances were as low as 0.001–0.005 and 0.005–0.01 μg L−1, respectively. The proposed method was employed to analyze urine samples which were pretreated with a protein precipitation process. The potential influences of precipitants on the analysis results were evaluated statistically, and 0.1% formic acid/acetonitrile/water was selected as the optimum precipitation agent. The detection of the targets was free from matrix and carryover effects.
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