CN110045053A - A kind of QuEChERS pre-treating method of the analysis of the amphetamines suitable for blood - Google Patents
A kind of QuEChERS pre-treating method of the analysis of the amphetamines suitable for blood Download PDFInfo
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- CN110045053A CN110045053A CN201910362999.7A CN201910362999A CN110045053A CN 110045053 A CN110045053 A CN 110045053A CN 201910362999 A CN201910362999 A CN 201910362999A CN 110045053 A CN110045053 A CN 110045053A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The invention discloses a kind of suitable for blood QuEChERS pre-treating method that amphetamines analyzes.This method is extracted reagent using QuEChERS and is effectively extracted to the amphetamines in blood, and composite packet purifies blood complex matrices, finally carries out pattern detection analysis.This method mainly includes the acquisition of blood sample, the extracting and developing of amphetamine and related substances, purification in blood.Blood sample amount required by the method for the invention at least can reach 0.2 mL, and minimum detection limit can be completed in 15 minutes up to 0.3 ~ 1.0 ng/ml, single sample pre-treatment.This method is easy to operate for the cytotoxic drug analysis method in blood sample, and consumed sample size is few, effectively eliminates matrix interference complicated in blood, and the rate of recovery greatly increases, and sensitivity significantly improves, and can be widely applied to legal medical expert's poisonous substance, forensic clinic detection.
Description
Technical field
The invention belongs to QuEChERS pre-treating method fields, and in particular to one kind amphetamines suitable for blood
The QuEChERS pre-treating method of analysis.
Background technique
Blood can accurately and timely reflect vivo medicine concentration and each drug as biological material most conventional in clinic
In the situation of target organ, and it is widely used in the multiple fields such as clinical monitoring, forensic toxicological analysis.In forensic toxicological analysis
In, mostly based on the blood sample of victim, to monitor the real-time blood concentration information for obtaining party.
Contain a large amount of organic matter in blood sample, wherein protein (hemoglobin, plasma proteins and enzyme and protide
Hormone), non-protein nitrogenous compound (nitrogen substance in blood other than isolating protein, mainly urea, uric acid, creatine, flesh
Acid anhydride, amino acid, ammonia, peptide, bilirubin), sugar and the organic matters such as other organic matters and vitamin, lipid (including steroid hormone)
It usually can also interfere with the analysis of object in instrument analysis.Pre-treating method is often the most frequently used side for eliminating matrix effect
Method, common Sample Pretreatment Technique has liquid-liquid extraction, precipitation of protein, solid phase extraction in toxicological analysis at present.Liquid liquid
Extraction is according to the difference of substance distribution coefficient in two kinds of immiscible liquid (such as water phase, organic phase), to reach extraction
The purpose take, separated.But liquid-liquid extraction must carry out under suitable pH value condition, so that the molecular state of determinand, therefore
It needs to adjust different pH value, limits its universal sample pre-treating method as system toxicological analysis.Albumen precipitation is logical
It crosses and the big organic solvent of different types of protein precipitant such as polarity (such as methanol, acetonitrile), acidic precipitation agent, inorganic is added
Salt, heavy metallic salt etc., to achieve the purpose that protein precipitation.Its advantages are that the pre-treatment for plasma sample does not select
Property, as long as sufficient amount can be measured.But the method for albumen precipitation is often examined the sample of low concentration and is not measured, this is right
In system toxicological analysis be a biggish deficiency because be easy to causeing the missing inspection of poisoning sample in this way.Solid Phase Extraction (SPE) can
Avoid in liquid-liquid extraction mutually separation not exclusively, be difficult to the disadvantages of automating, but solid phase procedures are more, handle relatively complicated, consumption
When it is longer.
SF/Z JD0107004-2016 " judicial expertise technical specification -- amphetamines, pethidine in biological material
With the measurement of ketamine " it is described, it takes blood sample 2mL to be placed in 10mL tool plug centrifuge tube, 10% sodium hydroxide solution is added
0.2mL is extracted, vortex mixed, centrifugation with ether 3mL, transfer organic layer to another centrifuge tube, is volatilized in about 60 DEG C of water-baths, residual
Stay addition 100uL acetonitrile in object: mobile phase buffer (70:30) is dissolved, and 5uL is taken to carry out LC-MS/MS analysis.With top
Method has the disadvantage in that (1) operating condition is stringent: liquid-liquid extraction must carry out under suitable pH value condition, so that determinand is in
Molecular state needs to adjust pH value in SF/Z JD0107004-2016.(2) inconvenient for operation: using after ether liquid-liquid extraction
Certain emulsion layer can be generated, is mutually separated not enough completely, the separation of supernatant layer takes liquid that can generate larger mistake because operator is different
Difference.(3) sample dosage is relatively more.
Summary of the invention
The object of the present invention is to provide a kind of suitable for blood the pre-treatment side QuEChERS that amphetamines analyzes
Method, this method can effectively extract the amphetamines related substances such as amphetamine, crystal methamphetamine, the head-shaking pill in blood sample, right
Complex matrices blood is purified, and eliminates matrix interference complicated in blood, so that the rate of recovery greatly increases, sensitivity is significantly mentioned
Height can be used for carrying out qualitative and quantitative analysis detection.
The purpose of the present invention is achieved through the following technical solutions.
A kind of QuEChERS pre-treating method of the analysis of the amphetamines suitable for blood, includes the following steps:
1) extraction reagent is added into blood to extract；The reagent that extracts is to be mixed with containing formic acid, methanol, acetonitrile
Machine reagent；
2) separation material packet, vortex mixed, centrifugation are added into mixed liquor obtained by step 1)；The separation material includes
Grinding bead and anhydrous magnesium sulfate；
3) it is centrifuged in gained supernatant to step 2) and the scavenging material packet containing C18 and PSA is added, stood, take after vortex
The excessively organic filter membrane of supernatant, filtered fluid carry out nitrogen and blow, and acetonitrile buffer is then added and redissolves upper machine.
Preferably, the dosage of the step 1) blood is 0.2~0.5mL.
Preferably, step 1) the extraction reagent is the acetonitrile extracting solution containing 10%~30% methanol.
Preferably, it is 10~30 parts that methanol volume in reagent is extracted with volume basis, in step 1), acetonitrile solvent is 70~
90 parts.
Preferably, it is 0.1% that formic acid volume ratio in reagent is extracted with volume basis, in step 1).
Preferably, with volume basis, the middle dosage for extracting reagent of step 1) is 1mL.
Preferably, the grinding bead is zirconium oxide abrasive pearl, is 3~10 in quantitative terms.
Preferably, separation material packet described in step 2) also contains Boratex, in terms of mass fraction, anhydrous magnesium sulfate 3
~5 parts, Boratex is 1~2 part.
Preferably, in step 2) the separation material packet, the dosage of anhydrous magnesium sulfate is 100~150mg, the use of Boratex
Amount is 20mg~50mg.
Preferably, the time of the step 2) vortex is 1 minute.
Preferably, the rate of the step 2) centrifugation is 3000r/min~5000r/min, further preferably 5000r/
min。
Preferably, the scavenging material packet, in terms of mass fraction, C18 is 1 part, and PSA is 2~3 parts；Further preferably
C18:PSA=1:2.
Preferably, the quality of step 3) the scavenging material packet is 30~50mg.
Preferably, the time of the step 3) vortex is 15s~60s, and the time of standing is 30s~90s.
Preferably, in step 3), sample crosses the organic filter membrane of 0.22um after standing.
Preferably, acetonitrile in the step 3) acetonitrile buffer: the volume ratio of ammonium acetate is 70:30~90:10.
Preferably, the dosage of the step 3) acetonitrile buffer is 50~200uL.
Preferably, in step 3), the sample after being dissolved in acetonitrile buffer is using the detection point of liquid chromatography mass combined instrument
Amphetamine substance is analysed, actual conditions are as follows:
A) liquid phase column: specification is 3 × 150mm, and 5 μm of Gemini chromatographic column connects pot strainer；
B) mobile phase: methanol-buffer, buffer are the solution of 20mmol/L ammonium acetate and 0.1vt% formic acid；
C) constant current: 350 μ L/min；
D) column temperature: 40 DEG C；
E) Mass Spectrometry Conditions:
Electrospray ionisation ion source (ESI), cation (MRM) detection pattern；Interface temperature: DL:280 DEG C；It is atomized temperature
It spends (TEM): 450 DEG C.
Compared with prior art, the present invention has the advantage that
(1) present invention optimizes improvement using QuEChERS method, carries out benzene using the big mixing organic reagent of polarity
The extraction of third amine drug, while improving extracting mode, grinding bead is added, so that extraction efficiency greatly increases；Since purification is wrapped
Addition so that complex matrices are significantly purified in blood, the macromoleculars such as phosphatide, protein preferably in removal blood
Object is closed, influence of the chaff interferent to target compound is reduced；Consumed sample size is small (only 0.2mL), and detection sensitivity reaches 0.3~
1.0ng/ml, single sample pre-treatment can be completed in 15 minutes.
(2) it is easy to operate to test established improvement QuEChERS method, can avoid newborn in traditional liquid-liquid extraction method
Change the appearance of layer, and reduces the human error in pipetting processes.
(3) present invention preferably, can be widely applied to analysis specificity between amphetamine and related nine kinds of substances
Legal medical expert's poisonous substance qualitative and quantitative analysis, for the use of law enforcement agency, government, testing department and drug control institutions.
Specific embodiment
Specific implementation of the invention is further described below in conjunction with example, but embodiments of the present invention are not limited to
This.
Embodiment 1
The present embodiment adds amphetamine, crystal methamphetamine, head-shaking pill MDA (3,4- methylenedioxy in negative blood
Amphetamine), MDMA (3,4- methylenedioxy crystal methamphetamine), MDEA (N- ethyl -3,4- methylenedioxyphenyl propylamine),
PMMA (to methoxy amphetamine), N- isopropyl benzylamine, Ephedrine (ephedrine), Selegiline (selegiline)
Nine kinds of standard items of equal amphetamines and its related substances.Sample extracted reagent obtained of subscripting is extracted into separation, purification, richness
LC/MS-MS analysis is carried out after collection.With each determinand peak area (Y) for ordinate, corresponding compound concentration (X, ng/mL) is cross
Coordinate carries out linear regression analysis.Continuous 5d standard curve calculates deviation, the linear correlation system of slope, intercept and related coefficient
Number.Compound concentration is respectively the standard addition sample of 100ng/mL and 400ng/mL, prepares 6 samples in each concentration on the same day
This, calculates concentration and CV value, determines the rate of recovery of method and in a few days detect precision；Continuous 5 days, the two concentration were prepared respectively
Standard adds sample, calculates CV value, determines the detection preci-sion and accuracy in the daytime of method.
One, experimental procedure:
(1) the tested sample blood of 0.2mL is taken respectively, and extraction reagent of the 1mL containing formic acid 0.1% is added, and (extracting reagent is
Acetonitrile: the volume ratio of methanol is the mix reagent of 70:30) it extracts at room temperature 1 minute, add 150mg anhydrous slufuric acid
Magnesium, 30mg Boratex, 4~6 grinding beads are vortexed 1 minute, are then centrifuged at 5000r/min, take supernatant.
(2) 30mg cleanser (C18:PSA=1:2) is added into supernatant, 60s is stood after vortex 30s, crossing 0.22um has
Machine filter film carries out nitrogen and blows, and is then redissolved, is placed in acetonitrile buffer (acetonitrile: the volume ratio of 20mmol/L ammonium acetate is 70:30)
In autosampler bottle containing interpolation pipe, analyzed for LC-MS-MS.
(3) liquid chromatography mass combined instrument is analyzed, and specific testing conditions are as follows:
A) liquid phase column: Gemini chromatographic column (3 × 150mm, 5 μm) connects pot strainer；
B) mobile phase: methanol-buffer, buffer are the solution of 20mmol/L ammonium acetate and 0.1vt% formic acid；
C) constant current: 350 μ L/min.
D) column temperature: 40 DEG C.
E) Mass Spectrometry Conditions
Electrospray ionisation ion source (ESI), cation (MRM) detection pattern；Interface temperature: DL:280 DEG C；It is atomized temperature
It spends (TEM): 450 DEG C.
Amphetamine and its related nine kinds of drugs added under three kinds of concentration under the rate of recovery, matrix interference rate such as 1 institute of table
Show, the precision under nine kinds of drugs of amphetamine and its correlation add under three kinds of concentration is as shown in table 2.
Table 1
Table 2
Embodiment 2
The present embodiment is 8 amphetamines substances such as amphetamine, crystal methamphetamine, head-shaking pill in suspicion human blood of being involved in drug traffic
Test experience example.
One, experimental procedure:
(1) it the acquisition of blood sample: takes the blood sample of tester to be placed in anticoagulant blood vessel, and is saved in 4 DEG C of refrigerators.Respectively
The tested sample blood of 0.2mL is taken, the extraction reagent (acetonitrile: methanol=70:30) that 1mL volume ratio containing formic acid is 0.1% is added,
It extracts at room temperature 1 minute, adds 150mg anhydrous magnesium sulfate, 30mg Boratex, 4~6 grinding beads are vortexed 1 point
Then clock is centrifuged at 5000r/min, takes supernatant.
(2) 30mg cleanser (C18:PSA=1:2) is added into supernatant, 30s~90s is stood after vortex 15s~60s,
The organic filter membrane progress nitrogen of 0.22um is crossed to blow, it is then multiple with acetonitrile buffer (acetonitrile: 20mmol/L ammonium acetate buffer=70:30)
It is molten, it is placed in the autosampler bottle containing interpolation pipe, is analyzed for LC-MS-MS.
(3) negative blood (normal human blood for being used as control) for taking 6 parts of 0.2mL, is added standard substance working solution,
It is made into the series of concentrations standard solution of 0,2.5,50,100,200,500ng/mL, is mixed；It is carried out through above-mentioned step (1)-(2)
It extracts, after purification, is analyzed to liquid chromatography mass combined instrument；
(4) to above-mentioned detected person's blood and negative blood after pre-treatment, liquid chromatography mass connection is carried out respectively
It is analyzed with instrument, specific testing conditions are as follows:
A) liquid phase column: Gemini chromatographic column (3 × 150mm, 5 μm) connects pot strainer；
B) mobile phase: methanol-buffer, buffer are the solution of 20mmol/L ammonium acetate and 0.1vt% formic acid；
C) constant current: 350 μ L/min.
D) column temperature: 40 DEG C.
E) Mass Spectrometry Conditions
Electrospray ionisation ion source (ESI), cation (MRM) detection pattern；Interface temperature: DL:280 DEG C；It is atomized temperature
It spends (TEM): 450 DEG C.
Two, data processing
(1) testing result of the series of concentrations standard solution according to made of negative blood draws normal concentration quantitation curves,
The specific method is as follows:
Using external standard method, with each determinand peak area (Y) for ordinate, corresponding compound concentration (X, ng/mL) is horizontal seat
Mark carries out linear regression analysis, is not forced through origin, carries out simple linear regression analysis, obtained regression equation is as follows, i.e.,
The linear equation of amphetamine and its related nine kinds of drugs, related coefficient and detection limit are as shown in table 3.
Table 3
(2) it according to gained quantitation curves and regression equation in the testing result of tester's blood and step (1), calculates
8 suspicion person's septicemia product contents are as shown in table 4.
Table 4
ND expression is not detected
The method of the present invention efficiently separates the amphetamines extracted in blood, and method is easy, sensitivity and accurate
Degree is high, while it can purify blood matrix, solves the problems, such as the matrix effect in analysis, high specificity, for political affairs
Mansion law enforcement agency, testing department and drug control institutions use.
Claims (10)
1. a kind of QuEChERS pre-treating method of the analysis of the amphetamines suitable for blood, which is characterized in that including such as
Lower step:
1) extraction reagent is added into blood to extract；The extraction reagent is the organic examination of mixing containing formic acid, methanol, acetonitrile
Agent；
2) separation material packet, vortex mixed, centrifugation are added into mixed liquor obtained by step 1)；The separation material includes grinding
Pearl and anhydrous magnesium sulfate；
3) it is centrifuged in gained supernatant to step 2 and the scavenging material packet containing C18 and PSA is added, stood after vortex, take supernatant
Organic filter membrane is crossed, filtered fluid carries out nitrogen and blows, and acetonitrile buffer is then added and redissolves upper machine.
2. the method according to claim 1, wherein the dosage of blood described in step 1) is 0.2 ~ 0.5mL.
3. the method according to claim 1, wherein extracting methanol body in reagent in step 1) with volume basis
Product is 10 ~ 30 parts, and acetonitrile solvent is 70 ~ 90 parts.
4. the method according to claim 1, wherein extracting formic acid body in reagent in step 1) with volume basis
Product is than being 0.1%.
5. the method according to claim 1, wherein separation material packet described in step 2 also contains Boratex,
In terms of mass fraction, anhydrous magnesium sulfate is 3 ~ 5 parts, and Boratex is 1 ~ 2 part.
6. the method according to claim 1, wherein the time of vortex described in step 2 is 1 minute；The centrifugation
Rate be the r/min of 3000 r/min ~ 5000.
7. the method according to claim 1, wherein the scavenging material packet, in terms of mass fraction, C18 1
Part, PSA is 2 ~ 3 parts.
8. the method according to claim 1, wherein the time of vortex described in step 3) be 15s ~ 60s, standing
Time is 30s ~ 90s.
9. the method according to claim 1, wherein acetonitrile in acetonitrile buffer described in step 3): ammonium acetate
Volume ratio is 70:30 ~ 90:10.
10. the method according to claim 1, wherein the sample after being dissolved in acetonitrile buffer is adopted in step 3)
Amphetamine substance is tested and analyzed with liquid chromatography mass combined instrument, actual conditions are as follows:
A) liquid phase column: specification is 3 × 150 mm, and 5 μm of Gemini chromatographic column connects pot strainer；
B) mobile phase: methanol-buffer, buffer are the solution of 20 mmol/L ammonium acetates and 0.1vt% formic acid；
C) constant current: 350 μ L/min；
D) column temperature: 40 DEG C；
E) Mass Spectrometry Conditions:
Electrospray ionisation ion source ESI, cation MRM detection pattern；Interface temperature: DL:280 DEG C；Atomization gas temperature TEM:450
℃。
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