Preparation method and application of fentanyl medicine hair standard substance
A standard substance, flufentanil technology, applied in the field of analytical chemistry, can solve the problem of not finding fentanyl drug standard substances, lack of detection standard substances, and lack of reliability, accuracy and traceability of test results. Safeguard and other issues, to achieve the effect of simple and fast sample pretreatment process, good accuracy and easy operation
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[0077] In the present invention, a preparation method of a fentanyl-type drug standard substance in a hair sample, the steps are as follows:
[0078] (1) Collect adult hair samples with no history of illegal drug use, wash the collected hair samples with pure water and chromatographic grade methanol three times each, dry at room temperature and cut them into 2cm pieces.
[0079] (2) Preparation of soaking solution: weighing acetylfentanyl, isobutyrylfentanyl, p-fluorofentanyl, orfentanyl, thiofentanyl, 4-fluorobutyrylfentanyl, tetrahydrofuranfentanyl, fentanyl Nine kinds of fentanyl-type drugs, fentanyl and desmethylfentanyl, were placed in a container, distilled water and dimethyl sulfoxide solution were added, and the mixture was uniformly mixed by ultrasonic, which was a drug-dimethyl sulfoxide solution.
[0080] GC-MS / MS for acetylfentanyl, isobutyryl fentanyl, p-flufentanyl, orfentanyl, thiofentanyl, 4-fluorobutyryl fentanyl, tetrahydrofuran fentanyl, fentanyl and Demeth...
Embodiment 1
[0104] Qualitative analysis and determination of purity of pure fentanyl-like drugs.
[0105] Acetylfentanyl, isobutyrylfentanyl, p-fluorofentanyl, orfentanyl, thiofentanyl, 4-fluorobutyrylfentanyl, tetrahydrofuranfentanyl, fentanyl and desmethylfentanyl which The pure raw materials of 9 kinds of fentanyl drugs were provided by the Physical Evidence Identification Center of the Ministry of Public Security, and were sealed and stored in a 4°C refrigerator after vacuum packaging. According to the gravimetric method, a single standard solution with high concentration was prepared using methanol as a solvent, and stored in a refrigerator. During the experiment, according to the analysis requirements, use methanol to dilute to the desired concentration.
[0106] GC-MS / MS was used to qualitatively analyze 9 kinds of pure fentanyl drugs. Instrument: Agilent 7890A-7000 Triple Quadrupole GC-MS; Chromatographic column: DB-5MS column (30m×0.25mm×0.25μm); Injection port temperature: 280...
Embodiment 2
[0111] Preparation of hair standards.
[0112]Weigh approximately 30mg of Acetylfentanyl, Isobutyrylfentanyl, p-Fluorfentanyl, Orfentanil, Thiofentanyl, 4-Fluorobutyrylfentanyl, THF, Fentanyl and Demethylfentanyl Fentanyl 9 fentanyl-like drugs are placed in 1000mL bottles. Add 500 mL of distilled water and 500 mL of dimethyl sulfoxide solution (containing 0.02 mol / L hydrochloric acid), ultrasonicate for 5 minutes to make them evenly mixed, and after cooling, soak 40 g of hair in it, and place it in the dark at room temperature. During the preparation of the hair standard material, a part of the samples were taken on the 7th day, the 15th day, the 20th day, the 22nd day, the 24th day, and the 25th day after soaking, respectively, and analyzed by LC-MS / MS. The results showed that within 7-22 days, the content of the drug increased with the soaking time, and when the soaking time reached 24 days, the highest concentration of the drug entered the hair. After soaking for 24 days,...
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