CN-122016983-A - Method for detecting multiple drugs in hair

CN122016983ACN 122016983 ACN122016983 ACN 122016983ACN-122016983-A

Abstract

The invention discloses a method for detecting multiple drugs in hair, which comprises the steps of S1, preparing drug stock solution by methanol, respectively diluting the drug stock solution into intermediate solutions with different concentrations, respectively adding quantitative intermediate solutions into equal blank hair extracting solutions to obtain standard hair extracting solutions with different concentration grades, S2, performing mass spectrum detection after solid phase extraction, performing linear regression on the standard concentration by using the signal intensity of quantitative ion mass spectrum peak to construct a standard curve, S3, cutting the hair to be detected, adding mixed solution, grinding the hair to be detected to powder, standing, taking supernatant fluid, filtering the supernatant fluid to be used as a hair extracting solution of a detection material, S4, performing solid phase extraction on the hair extracting solution, collecting the eluent, performing mass spectrum detection to obtain the quantitative ion peak signal intensity of the drug analyte, S5, comparing the standard curve, and calculating the concentration of the drug in a hair sample. The invention realizes on-site rapid screening and relatively higher detection accuracy and reliability.

Inventors

ZHANG YUNFENG
REN XINXIN
WEI CHUNMING
WANG RUIHUA
LI JIAYI
SONG GE
ZHOU GUANGJIN
Du Qiuyao
WANG HAIXING
ZOU BO
DONG LINPEI
ZHANG JIAN
WU JIAHUI
WU XIAOJUN
ZHAO PENG
CHANG JING

Assignees

公安部鉴定中心

Dates

Publication Date: 20260512
Application Date: 20260119

Claims (10)

1. A method for detecting multiple drugs in hair, comprising the steps of: s1, preparing a drug stock solution by using methanol, respectively diluting the drug stock solution into intermediate solutions with different concentrations by using the methanol, and respectively adding quantitative intermediate solutions into equal amounts of blank hair extract to obtain standard hair extract with different concentration levels; S2, carrying out mass spectrum detection on the labeled hair extracting solutions with different concentration levels after solid phase extraction, and carrying out linear regression on the labeled concentration by using the signal intensity of the quantitative ion mass spectrum peak to construct a standard curve; S3, cutting the hair to be detected, adding the cut hair into a mixed solution of methanol and water, grinding the cut hair into powder, and dispersing the powder; S4, performing solid-phase extraction on the hair extract of the detection material, wherein the solid-phase extraction adopts a mixed solution of ammonia water and methanol as an eluent, and performing mass spectrometry detection after collecting the eluent to obtain the signal intensity of a quantitative ion mass spectrometry peak of the drug analyte; S5, comparing the signal intensity of the quantitative ion mass spectrum peak of the drug analyte with a standard curve, and calculating the concentration of the drug in the hair to be detected.
2. The method for detecting multiple drugs in hair according to claim 1, wherein in S1, the drug stock solution is a mixed stock solution of methamphetamine, 3, 4-methylenedioxymethamphetamine, ketamine, norketamine, etomidate, ipratropium and 2- (ethylamino) -2-phenylcyclohexyl-1-one with the concentration of 5 mg mL -1 ; In S1, the preparation method of the blank hair extract comprises the steps of sequentially washing and drying blank hair which is detected to be negative through distilled water and methanol, cutting the blank hair, adding the cut blank hair into a mixed solution of the methanol and the water, grinding the cut blank hair into powder to obtain a dispersion liquid, standing the dispersion liquid, taking supernatant and filtering the supernatant through an organic microporous filter membrane to obtain the blank hair extract.
3. The method of claim 1, wherein in S3, the volume ratio of methanol to water in the mixed solution is 1:1.
4. The method for detecting multiple drugs in hair according to claim 1, wherein in S4, mass spectrometry detection analysis shows that the quantitative ion of methamphetamine is m/z 119,3,4-methylenedioxymethamphetamine is m/z 163, the quantitative ion of ketamine is m/z 207, the quantitative ion of norketamine is m/z 207, the quantitative ion of etomidate is m/z 141, the quantitative ion of isopropyl pamoate is m/z 155,2- (ethylamino) -2-phenylcyclohex-1-one is m/z 173.
5. The method for detecting multiple drugs in hair according to claim 1, wherein in S4, the solid phase extraction is performed by using a pipette filled with solid phase extraction filler, and the extraction method by using the pipette is that the pipette is immersed into the hair extract of the detection material, repeatedly sucking and discharging for several times, then washing with methanol, repeatedly eluting with a mixed solution containing ammonia water and methanol, and collecting supernatant for detection.
6. The method for detecting multiple drugs in hair according to claim 5, wherein the solid phase extraction filler adopted by the tip of the pipetting gun is MCX, the volume ratio of ammonia water to methanol in the mixed solution of ammonia water and methanol is 5:95, and the concentration of ammonia water is 25-28wt%.
7. The method of claim 1, wherein in S4, a micro mass spectrometer is used for mass spectrometry.
8. The method of claim 7, wherein the mass spectrometry is performed by using paper spray ionization.
9. The method of claim 8, wherein the ionization sample is injected with a spray voltage of 4200 v, a spray voltage of 3, 4-methylenedioxymethamphetamine of 4200V, a spray voltage of ketamine of 4100V, a spray voltage of norketamine of 4100V, a spray voltage of etomidate of 4400V, a spray voltage of isopropyl pamoate of 4400 v, and a spray voltage of 2- (ethylamino) -2-phenylcyclohex-1-one of 4100V.
10. The method for detecting multiple drugs in hair according to claim 8, wherein during ionization sample injection, the energy of ISO1 of methamphetamine is 7 v, the energy of ISO1 of 3, 4-methylenedioxymethamphetamine is 7V, the energy of ISO1 of ketamine is 8V, the energy of ISO1 of norketamine is 10V, the energy of ISO1 of etomidate is 9V, the energy of ISO1 of isopropyl pacifier is 9 v, and the energy of ISO1 of 2- (ethylamino) -2-phenylcyclohexyl-1-one is 10V; the energy of ISO2 of methamphetamine is 2.5 v, the energy of ISO2 of 3, 4-methylenedioxymethamphetamine is 3V, the energy of ISO2 of ketamine is 3.5V, the energy of ISO2 of norketamine is 3.5V, the energy of ISO2 of etomidate is 3V, the energy of ISO2 of isopropyl pamoate is 4 v, the energy of ISO2 of 2- (ethylamino) -2-phenylcyclohex-1-one is 4V; the energy of the CID of methamphetamine was 1V, the energy of the CID of 3, 4-methylenedioxymethamphetamine was 3.75V, the energy of the CID of ketamine was 1.75V, the energy of the CID of norketamine was 2.25V, the energy of the etomidate CID was 1.25V, the energy of the isopropyl midate CID was 1.25V, and the energy of the 2- (ethylamino) -2-phenylcyclohex-1-one CID was 1.5V.

Description

Method for detecting multiple drugs in hair Technical Field The invention relates to the technical field of drug detection in biological matrixes. In particular to a method for detecting various drugs in hair. Background In recent years, new mental active substances are layered endlessly, and drugs bring great threat to human health and social stability. The detection means of drugs is a necessary condition for striking new drugs and new psychoactive substances which are endless at the present time, and the requirements for on-site rapid screening of the involved people are increasing. However, the existing drug detection methods based on biological fluids such as urine and blood depend on laboratory analysis, have the limitations of complex pretreatment, long detection period, incapability of being separated from a fixed laboratory and the like, and are difficult to meet the urgent demands of site searching work on timeliness and convenience. This contradiction is particularly pronounced in trace drug detection, where complex biological matrices severely interfere with the accuracy and reliability of the detection. Therefore, developing a detection technology capable of being used in a field environment to realize rapid and accurate screening of various drugs in biological fluids has become an urgent need in the field of detoxification practice. Disclosure of Invention Therefore, the technical problem to be solved by the invention is to provide a method for detecting various drugs in hair, which is simple to operate, realizes on-site rapid screening, and simultaneously realizes relatively higher detection accuracy and reliability. In order to solve the technical problems, the invention provides the following technical scheme: a method for detecting multiple drugs in hair, comprising the following steps: s1, preparing a drug stock solution by using methanol, respectively diluting the drug stock solution into intermediate solutions with different concentrations by using the methanol, and respectively adding quantitative drug stock solutions into equivalent blank hair extract to obtain standard hair extract with different concentration levels; S2, carrying out mass spectrum detection on the labeled hair extracting solutions with different concentration levels after solid phase extraction, and carrying out linear regression on the labeled concentration by using the signal intensity of the quantitative ion mass spectrum peak to construct a standard curve; S3, cutting the hair to be detected, adding the cut hair into a mixed solution of methanol and water, grinding the cut hair into powder, and dispersing the powder; s4, performing solid-phase extraction on the hair extract of the detection material, wherein the solid-phase extraction adopts a mixed solution of ammonia water and methanol as an eluent, and performing mass spectrometry detection after collecting the eluent to obtain the signal intensity of a quantitative ion mass spectrometry peak of the drug analyte; S5, comparing the signal intensity of the quantitative ion mass spectrum peak of the drug analyte with a standard curve, and calculating the concentration of the drug in the hair to be detected. According to the application, the hair is crushed, ground into powder in a mixed solution of methanol and water, then the powder is dispersed, the dispersion is kept stand and filtered by an organic microporous filter membrane, and solid phase extraction elution is carried out by adopting a mixed solution of ammonia water and methanol (the volume ratio of the ammonia water to the methanol is 5:95) as an eluent and MCX as a filler, so that the target object is efficiently recovered. The purification steps effectively remove complex matrix interferences such as lipid, protein and the like in the hair, obviously reduce the ion inhibition effect possibly generated on a target object in the ionization process, improve the ionization efficiency, thereby enhancing the signal intensity of mass spectrum, enabling preliminary quantification to be carried out without using an internal standard method, realizing rapid preliminary screening of a hair sample, realizing relatively higher detection accuracy and reliability of various drugs in the hair, and the synergy of the treatment steps fundamentally solves the technical problems of high-efficiency release and purification of drug molecules from compact hair keratin matrix, and lays a foundation for subsequent high-efficiency ionization. Firstly, the specific surface area of a sample is greatly increased through wet grinding, the hair structure is thoroughly destroyed, drug molecules embedded in the hair structure are fully dissolved out, namely the drug molecules are efficiently extracted into a solvent, so that the ion quantity of a final object to be detected is remarkably improved, and the target object can be prevented from being degraded due to overheat of the system through wet grinding. And finally, when the puri