Detection method of new psychoactive substance BZP
A detection method and mass spectrometry technology are applied in the detection field of the new psychoactive substance BZP, which can solve the problems of complex biological sample matrix, troublesome detection work, and many interferences, and achieve the advantages of analytical operation, efficient qualitative and quantitative analysis, and high sensitivity. Effect
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Embodiment 1
[0074] Embodiment 1, GC-MS detects BZP in the urine sample
[0075] (1) Preparation of sample solution
[0076] An Oasis HLB solid phase extraction cartridge (60 mg, 3 mL) was first pretreated with 2 mL of methanol, 2 mL of deionized water and 2 mL of ammonium acetate (10 mM, pH=9.5). After sample loading, the solid-phase extraction cartridge was washed with 1 mL of deionized water, and then dried in vacuum. Elute with 1 mL of methanol, blow to dryness with nitrogen, redissolve with methanol to 400 μL, filter and centrifuge, and put into a sample vial.
[0077] (2) Setting of detection conditions
[0078] The setting process of gas chromatography conditions is as follows:
[0079] The carrier gas is helium;
[0080] Chromatographic column is DB-5MS or HP-5MS;
[0081] The heating program is as follows: the initial temperature is 70°C, rising to 300°C at a rate of 10°C / min, and keeping for 7 minutes;
[0082] Mass spectrometry conditions: the voltage scanning range is set...
Embodiment 2
[0086] Embodiment 2, gas chromatography detects the BZP in the hair
[0087] (1) Preparation of sample solution
[0088] Basically the same as in Example 1.
[0089] (2) Preparation of standard working solution
[0090] Take the BZP standard stock solution and dilute it sequentially into a series of standard solutions with mass concentrations of 1.0, 0.5, 0.25, 0.125, 0.1, 0.05, 0.01, 0.005, and 0.001 mg / mL.
[0091] Take 1 μL of standard solutions of different concentrations and inject them, and record the corresponding peak area.
[0092] Each concentration was injected 3 times, and linear regression was performed on the average A of the 3 peak areas and the mass concentration c (mg / mL) to obtain the regression equation of BZP: A=622.26c+0.0716, r 2 It is 0.9966, the linear range is 5~1000μg / mL, and the detection limit is 5μg / mL (S / N≥3).
[0093] (3) Setting of detection conditions
[0094] The carrier gas is nitrogen;
[0095] Chromatographic column is DB-5 or HP-5; ...
Embodiment 3
[0107] Embodiment 3, liquid chromatography detects BZP in blood
[0108] (1) Preparation of sample solution
[0109] Basically the same as in Example 1.
[0110] (2) Preparation of standard working solution
[0111] Take the BZP standard stock solution and dilute it sequentially into a series of standard solutions with mass concentrations of 1.0, 0.75, 0.5, 0.1, 0.05, 0.025, 0.01, 0.005, 0.001, and 0.0005 mg / mL.
[0112] Take 10 μL of standard solutions of different concentrations and inject them, and record the corresponding peak area.
[0113] Each concentration was injected 3 times, and linear regression was performed on the average A of the peak area of the 3 times and the mass concentration c (mg / mL), and the regression equation of BZP was A=89079c+117849, r 2 =0.999 6, the linear range is 5-1000 μg / mL, the limit of quantification is 5 μg / mL (S / N≥3).
[0114] (3) Setting of detection conditions
[0115] The column is 300SB-C18 (4.6×150mm, 5μm);
[0116] The colu...
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