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(2) Extraction method
1) Barbiturates
Acetonitrile and ethyl acetate are the most commonly used organic solvents in the extraction of barbiturates
Dai Xiaoxin et al.
Barbiturates are acidic and exist in a molecular state under acidic conditions.
Industry standards of inspection and quarantine SNT 2217-2008 chicken extract, pork, liver and fish with an acidic acetonitrile phenobarbital , pentobarbital , amobarbital and secobarbital six kinds of barbituric Class drugs, determined by LC-MSMS, the method LOD is 1 μg/kg, and the recovery rate is 78.
2) Benzodiazepines
Benzodiazepines are mainly extracted with organic solvents such as acetonitrile and ethyl acetate
Determination of 12 Gunn et benzodiazepine class of drugs in serum and whole blood (including alprazolam , temazepam , oxazepam , nordiazepam , clonazepam , lorazepam , diazepam , Lee For Mianning , midazolam , flunitrazepam , 7-aminoclonazepam and 7-aminoflunazepam), use 4℃ cold acetonitrile to precipitate the protein, vortex extraction, and change the solvent of the extract to super high efficiency Liquid chromatography tandem mass spectrometry (UPLC-MS/MS) analysis
Huang Shixin et al.
Xie Xiuhong et al.
3) Phenothiazines
The polarity of phenothiazine drugs is quite different.
Cheng et al.
Holland et al.
Zhu Li et al.
4) Butyrylbenzenes
Butyrylbenzene drugs are all alkaline, and the residual extraction also selects appropriate solvent extraction according to polarity and acidity and alkalinity
Cerkvenik-Flajs et al.
Aoki et al.
5) Simultaneous extraction of multiple types
Simultaneous extraction and determination of multiple sedative drugs greatly improves the detection efficiency
Chang Qing et al.
established barbital, pentobarbital, phenobarbital, oxazepam, diazepam, nitrazepam, clonazepam, estazolam, alprazolam and alprazolam in body fluids.
The qualitative and quantitative analysis method of triazolam
.
After the plasma sample was alkalized with 0.
1 mol/L sodium hydroxide solution, it was extracted with ethyl acetate, the extract was blown dry with nitrogen, and then dissolved with ethyl acetate for GC-MS analysis
.
The recovery rates of the 10 drugs were all between 92% and 117%, the intra-day and inter-day RSD were between 4.
09% and 14.
26%, and the LOD was between 2 and 20 μg/L
.
Bock et al.
developed a method using LC-MS/MS to determine the sedative azaperone and its metabolites azaperone, chlorpromazine, propionylpromazine and acepromazine, haloperidol and toluene in pig and cattle kidneys.
Methods of thiazide and other drugs
.
Using pig kidneys as contaminated animal samples, different types of solvents, extraction and purification methods have been tested and verified
.
The method with the highest extraction rate is to use a mixture of ammonia and ethyl acetate, shaking extraction, without solid phase extraction purification
.
Mitrowska et al.
used acetonitrile to extract phenothiazines such as chlorpromazine, propionylpromazine, acepromazine, triflupromazine, and drug residues of azaperone and azaperol in pig and bovine kidneys
.
After the extract was purified with a C18 solid phase extraction column, it was determined by LC-MS/MS
.
The method recovery rate is 73.
2%~110.
6%, CV is less than 13.
0%; CCa is: phenothiazines 5.
8~6.
6μg/kg, azaperone 105.
5μg/kg, azaperone 121.
4μg/kg, CCβ is: Phenothiazines 6.
3~7.
6μg/kg, azaperone 119.
0μg/kg, azaperol 140.
0μg/kg
.
Zhang et al.
used acetonitrile to simultaneously extract 11 sedatives (phenobarbital, estazolam, midazolam, diazepam, nitrazepam, defluphenazine, chlorpromazine, acepromazine, Haloperidol, xylazine, azaperol)
.
By comparing methanol, acetonitrile and ethyl acetate as the extraction liquid, it is found that acetonitrile has the best extraction effect, less impurities, and the highest recovery rate
.
The drug recovery rate in pig, bovine muscle, kidney and liver is between 76.
49% and 118.
6%, the CV is between 2.
2% and 19.
9%, and the LOQ is between 0.
5 and 2.
0 μg/kg
.