Extraction and detection method for ketamine, norketamine and amphetamin-type substances in hairs
An extraction method and methylketamine technology are applied to the extraction of norketamine and amphetamine-like substances, and the field of ketamine in hair can solve the problems of high price, severe conditions, long acid hydrolysis time, etc., and achieve improved detection sensitivity and mild reaction conditions. , the effect of simple operation
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Embodiment 1
[0035] In this example, ketamine, norketamine and amphetamines (amphetamine, methamphetamine, MDMA, MDEA, MDA, methcathinone, 4-methyl methcathinone) are added to the negative hair, and pretreated by the compound solution , solid phase extraction, and derivatization for GC / MS-SIM analysis. Prepare 6 samples for each concentration on the same day, measure the ratio of each component to the peak area of the internal standard, calculate the recovery rate and CV value, and determine the recovery rate of the method and the precision of the intraday detection; for 5 consecutive days, prepare these two samples respectively The concentration standard is added to the sample, the ratio of each component to the peak area of the internal standard is measured, and the CV value is calculated to determine the day-to-day detection precision and accuracy of the method.
[0036] 1. Experimental steps:
[0037] (1) Weigh about 30 mg of negative hair, wash with 3 mL of detergent, water, and ...
Embodiment 2
[0055] This example is the standard substance of ketamine, norketamine and amphetamines in negative hair, which is pretreated with composite solution, solid phase extraction, and then analyzed by liquid chromatography mass spectrometry. Six parallel samples were prepared respectively at two concentration levels of 15000pg / mg and 80000pg / mg, and the recoveries were calculated.
[0056] 1. Experimental steps:
[0057] (1) Weigh about 40 mg of negative hair respectively, and the cleaning and freezing grinding process is the same as that in Example 1;
[0058] (2) Accurately weigh 30 mg of ground negative hair powder, add 2 mL of hair compound treatment solution (the specific components are 0.3 mol / L phosphate buffer solution, 0.5% bovine serum albumin, 3% Tween, and Adjust the pH value to 2.0), add an internal standard, sonicate at 85°C for 2 hours, and centrifuge to obtain the supernatant;
[0059] (3) The equilibration, sample loading, and washing process of the solid phase e...
Embodiment 3
[0075] This embodiment is an experimental example of detection of ketamine, norketamine and amphetamines (such as amphetamine, methamphetamine, MDMA) in the hair of 8 drug abusers.
[0076] 1. Experimental steps:
[0077] (1) Weigh about 30 mg of the hair of the abuser, wash it with 3 mL of detergent, water, and acetone, cut it into 1.0 mm segments, and grind it with liquid nitrogen to obtain the ground hair powder;
[0078] (2) Accurately weigh 20 mg of the abuser's hair powder after grinding, and add 2 mL of hair compound treatment solution (the specific components are 0.1 mol / L phosphate buffer solution, 1% bovine serum albumin, 3% Tween, and its pH value was adjusted to 2.7), adding an internal standard, ultrasonicating at 70°C for 4 hours, and centrifuging to obtain a supernatant;
[0079] (3) Equilibrate the solid-phase extraction column with 1mL methanol, 1mL water, and 1mL 0.1M phosphate buffer in sequence, and inject the above hair pretreatment supernatant, wash impu...
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