This paper aims to establish a solid-phase support liquid-liquid extraction-high performance liquid chromatography/triple quadrupole tandem mass spectrometry (SLE-HPLC-MS/MS) method for the detection of scopolamine, anisodamine and atropine in blood and urine. The effects of protein precipitated method, solid phase extraction method and solid-phase supported liquid-liquid extraction method on the extraction of drugs from blood and urine samples were investigated. Scopolamine, anisodamine and atropine, in blood and urine samples were analyzed by high performance liquid chromatography triple quadrupole tandem mass spectrometry. The results showed that the recovery rate of solid-phase supported liquid-liquid extraction was the highest. The linear relationship between the concentration of scopolamine, anisodamine and atropine in blood and urine and the peak area (r>0.9992) was good in the range of 0.1－100 ng/mL (blood) and 0.5－100 ng/mL (urine). The minimum detection limit of scopolamine, anisodamine and atropine in blood was 0.01 ng/mL, and the quantitative limit was 0.1ng/mL; The minimum detection limit of scopolamine, anisodamine and atropine in urine was 0.05 ng/mL, and the quantification limit was 0.5 ng/mL. The solid-phase supported liquid-liquid extraction liquid chromatography/tandem mass spectrometry method is characterized by simple operation, less solvent usage and high recovery rate. It is suitable in the detection of scopolamine, anisodamine and atropine in blood and urine for three types of drug poisoning cases (incidents).

A method was developed for the determination of etomidate and its metabolite etomidate acid in hair and urine by high performance liquid chromatography-triple quadrupole tandem mass spectrometer (HPLC-MS/MS). The hair samples were ground and extracted by ultrasonic extraction with methanol. After protein was precipitated by acetonitrile, the urine samples were centrifuged at high speed and passed through 0.22 μm filter membrane, and then Agilent Eclipse Plus C18 RRHD (3.0 mm×150 mm×1.8 μm) column was used for analysis. Gradient elution was performed with 0.1% formic acid aqueous solution-acetonitrile as mobile phase at the flow rate of 0.5 mL/min. Electrospray ion source and multiple reaction monitoring (MRM) positive ion mode were selected. The results showed that the linear relationship of the two compounds exhibited good linearity in the concentration range of 0.5 to 50 ng/mL in urine and 0.025 to 2.5 ng/mg in hair, and the R² value was greater than 0.9925. The extraction recoveries ranged from 91.0% to 107.5%, and the intra-day and inter-day precision RSD was 0.4% to 7.4%, while the intra-day and inter-day accuracy was 91.5% to 110.8%. In the actual cases, six hair samples and 4 urine samples were tested, and the test results showed that etomidate was detected in all six hair samples, and the metabolite etomidate acid was detected in two hair samples, but the concentration was much lower than the original. Etomidate and metabolite etomidate acid were detected in two urine samples, and the metabolite concentration was much higher than the original. In conclusion, this method can be used for rapid qualitative and quantitative analysis of etomidate and its metabolite in the hair and urine of etomidate users.

The distribution and degradation of the synthetic cannabinoid ADB-BUTINACA of alkyl formyl indazoles in rats were explored in this paper. Through previous animal studies, it was found that the metabolic markers of ADB-BUTINACA in rats were dealkylation metabolic markers: N-(1-aminoformyl-2,2-dimethylpropyl)-indazole-3-formamide (hereinafter referred to as A1) and hydrolytic metabolic marker: 3,3-dimethyl-2- [1-Butyl-1H-indazole-3-formamido] butyric acid (hereinafter referred to as A2). An intoxication model of rat administered with ADB-BUTINACA by gavage established by simulating oral administration of cannabis products, and the concentration of ADB-BUTINACA and metabolic markers A1 and A2 in tissues, blood, urine and feces were detected by high performance liquid chromatography-triple quadrupole tandem mass spectrometry (HPLC-MS/MS), and the distribution and degradation of ADB-BUTINACA and metabolic markers in rats were monitored. The results showed that ADB-BUTINACA was rapidly metabolized and distributed in various tissues and blood after entering the rat body, and showed different regularity of distribution and degradation within 12 hours. In the monitoring of urine and feces collected within 1 to 10 days, ADB-BUTINACA and its metabolic markers were detected only in a small amount of urine, while they were all detected in feces collected within 24 to 72 hours. The rat intoxication model established in this study monitors the distribution and degradation of ADB-BUTINACA and metabolic markers in rats, providing scientific basis and data reference for the test of ADB-BUTINACA in vivo.