CN104820042A - Method for determining contents of cathinone and 4-methyl methcathinone in sample through high performance liquid chromatography - Google Patents
Method for determining contents of cathinone and 4-methyl methcathinone in sample through high performance liquid chromatography Download PDFInfo
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Abstract
The invention discloses a method for determining contents of cathinone and 4-methyl methcathinone in a sample through high performance liquid chromatography. The method comprises the following steps: preparing a working solution; (2) preparing a sample solution; (3) setting detection conditions; and (4) determining the contents of cathinone and 4-methyl methcathinone in a sample. According to the method, reversion phase chromatographic isocratic elution is used for separating cathinone and 4-methyl methcathinone within 10min; the method disclosed by the invention can provide efficient and accurate detection results and can be used for determining the contents of cathinone and 4-methyl methcathinone in the sample at the same time, thereby providing evidences for conviction and punishment of judicial departments.
Description
Technical field
The present invention relates to illicit drugs inspection field, criminal investigation field, particularly adopt the method for Cathinone and 4-methyl methcathinone content in high effective liquid chromatography for measuring sample.
Background technology
4-methyl methcathinone (Mephedrone) is a kind of spiritual material, belongs to the western ketones derivant of Synthesis Card, and its chemical structural formula is such as formula shown in (1):
Cathinone (Cathinone), have another name called benzoylethanamine (being hagigat again on Israel market), it is a kind of monoamine alkaloid (monoaine alkaloid) found in khat (khat), chemically having similarly: ephedrine (ephedrine), cathidine (cathine) and other pacify his unnatural death, its chemical structural formula is such as formula shown in (2):
Cathinone can cause dopamine D_2 receptors, may be khat to be produced stimulate sex reason.The Cathinone of Prof. Du Yucang, also often by the important component part as recreational drug, is called bath salt usually in the U.S..
Cathinone and 4-methyl methcathinone have suitable harm to human body.This harm not only affects the physiological situation of human body, also can affect the psychological activity of people, excessively also can cause death.The abuse of Cathinone and 4-methyl methcathinone not only has harm to human body, and also can cause adverse effect to the development of society.
Prior art has Cathinone and 4-methyl methcathinone content in working samples such as adopting gas chromatography/mass spectrometry method, infrared spectroscopy, high performance liquid chromatography and LC-MS technology.Wherein, in the process detected utilizing liquid phase chromatography, because both structures of matter are similar to, in order to be effectively separated by two materials, prior art adopts the mode reducing flow velocity usually, and this just causes detection time long, the technical matters that detection efficiency is low, makes criminal investigation work efficiency reduce.Therefore be badly in need of a kind of high-precision, and the method that in sample, Cathinone and 4-methyl methcathinone detect simultaneously can be realized in shorter time.
Summary of the invention
In view of this, the invention reside in the method that Cathinone and 4-methyl methcathinone content in a kind of precision is high, detection time is short hplc simultaneous determination sample are provided.
The present invention is achieved through the following technical solutions: a kind of method adopting Cathinone and 4-methyl methcathinone content in high effective liquid chromatography for measuring sample, it comprises the steps:
(1) preparation of working fluid;
(2) preparation of sample solution;
(3) setting of testing conditions;
(4) mensuration of Cathinone and 4-methyl methcathinone content in sample;
(5) experimental result calculates,
Wherein, in step (3), chromatographic column adopts anti-phase phenyl chromatographic column, and mobile phase is A-1 ~ 5mM ammonium acetate buffer: B-acetonitrile, A:B=(20 ~ 40): (60-80), and flow velocity is 1.0-1.5mL/min.
In the step (3) of said method, in step (3), the 4mM ammonium acetate buffer of A-pH=5.0: B-acetonitrile, A:B=20:80, flow velocity is 1.2mL/min.
Said method adopts inner mark method ration, selects 2-phenyl ethylamine as internal standard compound matter.
In the step (1) of said method, get Cathinone and 4-methyl methcathinone Standard Stock solutions respectively, by mass concentration be respectively the solution of the internal standard compound matter of 0.1mg/mL be diluted to successively Cathinone and 4-methyl methcathinone mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, two series standard solution of 0.0005mg/mL, and keep the concentration of inner mark solution to be 0.01mg/mL.
In the step (2) of said method: take sample, add mobile phase and dissolve, vibration, centrifugal, get supernatant after centrifugal, add internal standard compound matter, and add mobile phase, after shaken well, namely obtain sample solution; Mobile phase is identical with the mobile phase in step (3).
Said method adopts quantified by external standard method, wherein, in step (1), get Cathinone, 4-methyl methcathinone Standard Stock solutions respectively, be diluted to successively respectively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the two series standard solution of 0.0005mg/mL.
In the step (2) of said method: take sample, add mobile phase and dissolve, vibration, centrifugal, get supernatant after centrifugal, add mobile phase, after shaken well, namely obtain sample solution; Mobile phase is identical with the mobile phase in step (3).
In the step (3) of said method, chromatographic column specification is 250mm × 4.6mm, and 5 μm, column temperature is 35 DEG C, determined wavelength 254nm.
In said method, mobile phase puts into the ultrasonic 10 ~ 15min of ultrasonic cleaner before using after 0.45 μm of micro porous filtration membrane filtration, fully deviates from the gas in mobile phase.
Said method, before add mobile phase in sample, use the Cathinone in the mixed solution extraction sample of toluene, methyl phenyl ethers anisole, methylene chloride and ether or 4-methyl methcathinone, the volume ratio of toluene, methyl phenyl ethers anisole, methylene chloride and ether is 6:3:2:1.5, in isolated organic phase, add the hydrochloric acid that HCl massfraction is 20%, after removing organic phase residue is placed in 35 DEG C of rapid concentration instrument are concentrated into dry.
The invention has the beneficial effects as follows:
1) in prior art, because Cathinone is close with 4-methyl methcathinone structure, therefore be difficult to be separated in chromatogram detects, in order to ensure obtaining good degree of separation, often can only take the mode reducing flow velocity, improve degree of separation, improve peak shape, cause the detection time of Cathinone and 4-methyl methcathinone total material usually more than 30 minutes, and inventor is found by lot of experiments, it is improper that the principal element causing detection time in prior art long is that acid modification agent in mobile phase is selected, organic phase ratio can not be too high, by screening a large amount of modifier, inventor finds when using acidic ammonium acetate damping fluid, can by increasing organic phase ratio, greatly shorten detection time, the effective separation of test substance Cathinone and 4-methyl methcathinone can also be guaranteed simultaneously, the technique effects such as high theoretical cam curve, proved by test, the disengaging time of Cathinone and 4-methyl methcathinone can be foreshortened to about 10 minutes by the present invention, nearly the prior art used time 1/3rd, greatly improve detection efficiency, for effectively carrying out of criminal investigation work in reality provides powerful guarantee.
2) present invention employs inner mark method ration, compared to quantified by external standard method of the prior art, because internal standard method avoids because the accidental error that effect causes discriminated against by the consistance of sample introduction and sample, thus, its analytical precision is higher, is a kind of more satisfactory quantitative analysis method; Wherein, the determination of internal standard compound matter kind is one of difficult point marked in setting up in analytical approach, internal standard compound kind will directly affect degree of accuracy, the accuracy of testing result, interior mark selection is improper will directly cause detection to realize, inventor passes through lot of experiments, determine that 2-phenyl ethylamine is as internal standard compound matter, itself and Cathinone and 4-methyl methcathinone all have good degree of separation, achieve the accurate quantification of Cathinone and 4-methyl methcathinone.
Accompanying drawing explanation
Fig. 1 is the liquid chromatogram (horizontal ordinate-min, ordinate-mAU) of Cathinone and 4-methyl methcathinone, 1: Cathinone, 2:4-methyl methcathinone, 3: interior mark.
Embodiment
Embodiment 1
The present invention adopts the method for Cathinone and 4-methyl methcathinone content in high effective liquid chromatography for measuring sample, comprises the steps:
(1) preparation of working fluid; Get Cathinone and 4-methyl methcathinone Standard Stock solutions respectively, by mass concentration be respectively the solution of the internal standard compound matter of 0.1mg/mL be diluted to successively Cathinone and 4-methyl methcathinone mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, two series standard solution of 0.0005mg/mL, and keep the concentration of inner mark solution to be 0.01mg/mL.
(2) preparation of sample solution: the sample sample taken respectively containing Cathinone and 4-methyl methcathinone is about 45mg, and (the sample sample of the present embodiment prepares after using Cathinone standard items and 4-methyl methcathinone to mix with other material respectively, in sample one, Cathinone content is 49.86wt%, in sample two, 4-methyl methcathinone content is 50.42wt%), add 20mL mobile phase with bottleneck pipettor respectively to extract, vibrate 10 minutes, centrifugal 5 minutes, centrifugally use 1mL pipettor Aspirate supernatant 1mL respectively afterwards, add about 0.1mg internal standard compound matter 2-phenyl ethylamine respectively, and add 10mL mobile phase respectively with bottleneck pipettor, get 1.5mL after shaken well and fill auto injection bottle, namely sample solution is obtained,
(3) setting of testing conditions: adopt Agilent
sB-Phenyl chromatographic column, specification is 250mm × 4.6mm, 5 μm, the 4mM ammonium acetate buffer of chromatographic condition: A-pH=5.0: in B-acetonitrile=20:80[the present invention, ammonium acetate buffer calculates with the concentration of acetate, and 4mM is 4mmol/L, the ratio of ammonium acetate buffer solution and acetonitrile is volume ratio], flow velocity 1.2mL/min, column temperature 35 DEG C, determined wavelength 254nm;
(4) mensuration of Cathinone and 4-methyl methcathinone content in sample, respectively extracting sample solution 5 μ L sample detection;
(5) experimental result calculates, and utilize inner mark method ration to calculate, finally obtaining Cathinone content in sample one is 48.75wt%, and in sample two, 4-methyl methcathinone content is 49.27wt%.
Wherein, mobile phase puts into the ultrasonic 10 ~ 15min of ultrasonic cleaner before using after 0.45 μm of micro porous filtration membrane filtration, fully deviates from the gas in mobile phase.
Result shows, and Cathinone and 4-methyl methcathinone can separate completely, and peak shape is better, and liquid chromatogram as shown in Figure 1.
Embodiment 2
The present invention adopts the method for Cathinone and 4-methyl methcathinone content in high effective liquid chromatography for measuring sample, comprises the steps:
(1) preparation of working fluid; Get Cathinone, 4-methyl methcathinone Standard Stock solutions respectively, be diluted to successively respectively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the two series standard solution of 0.0005mg/mL.
(2) preparation of sample solution: the sample sample taken respectively containing Cathinone and 4-methyl methcathinone is about 45mg, and (the sample sample of the present embodiment prepares after using Cathinone standard items and 4-methyl methcathinone to mix with other material respectively, in sample one, Cathinone content is 49.86wt%, in sample two, 4-methyl methcathinone content is 50.42wt%), add 20mL mobile phase with bottleneck pipettor respectively to extract, vibrate 10 minutes, centrifugal 5 minutes, centrifugally use 1mL pipettor Aspirate supernatant 1mL respectively afterwards, 10mL mobile phase is added respectively with bottleneck pipettor, get 1.5mL after shaken well and fill auto injection bottle, namely sample solution is obtained,
(3) setting of testing conditions: adopt Agilent
sB-Phenyl chromatographic column, specification is 250mm × 4.6mm, 5 μm, the 4mM ammonium acetate buffer of chromatographic condition: A-pH=5.0: B-acetonitrile=20:80, flow velocity 1.2mL/min, column temperature 35 DEG C, determined wavelength 254nm;
(4) mensuration of Cathinone and 4-methyl methcathinone content in sample, respectively extracting sample solution 5 μ L sample detection;
(5) experimental result calculates, and utilize quantified by external standard method to calculate, finally obtaining Cathinone content in sample one is 48.39wt%, and in sample two, 4-methyl methcathinone content is 49.07wt%.
Wherein, mobile phase puts into the ultrasonic 10 ~ 15min of ultrasonic cleaner before using after 0.45 μm of micro porous filtration membrane filtration, fully deviates from the gas in mobile phase.
Result shows, and Cathinone and 4-methyl methcathinone can separate completely, and peak shape is better.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: specimen in use one is the blood of 49.86wt% for Cathinone content, namely gets blank blood, adds Cathinone standard items; Specimen in use two is 4-methyl methcathinone content is the blood of 50.42wt%, namely gets blank blood, adds 4-methyl methcathinone standard items.Toluene is added respectively in sample one and sample two, methyl phenyl ethers anisole, the mixed solution 25mL of methylene chloride and ether, Cathinone in extraction sample and 4-methyl methcathinone, toluene, methyl phenyl ethers anisole, the volume ratio of methylene chloride and ether is 6:3:2:1.5, the hydrochloric acid 20mL that HCl massfraction is 20% is added in isolated organic phase, after removing organic phase residue is placed in 35 DEG C of rapid concentration instrument are concentrated into dry, add 20mL mobile phase with bottleneck pipettor respectively to extract, vibrate 10 minutes, centrifugal 5 minutes, centrifugally use 1mL pipettor Aspirate supernatant 1mL respectively afterwards, add about 0.1mg internal standard compound matter 2-phenyl ethylamine respectively, and add 10mL mobile phase respectively with bottleneck pipettor, get 1.5mL after shaken well and fill auto injection bottle, namely sample solution is obtained.It is 48.25wt% that the present embodiment finally obtains Cathinone content in sample one, and in sample two, the content of 4-methyl methcathinone is 48.85wt%.
Embodiment 4
The difference of the present embodiment and embodiment 2 is: specimen in use one is the blood of 49.86wt% for Cathinone content, namely gets blank blood, adds Cathinone standard items; Specimen in use two is 4-methyl methcathinone content is the blood of 50.42wt%, namely gets blank blood, adds 4-methyl methcathinone standard items.Toluene is added respectively in sample one and sample two, methyl phenyl ethers anisole, the mixed solution 25mL of methylene chloride and ether, extract the Cathinone in sample and 4-methyl methcathinone respectively, toluene, methyl phenyl ethers anisole, the volume ratio of methylene chloride and ether is 6:3:2:1.5, the hydrochloric acid 20mL that HCl massfraction is 20% is added in isolated organic phase, after removing organic phase residue is placed in 35 DEG C of rapid concentration instrument are concentrated into dry, add 20mL mobile phase with bottleneck pipettor respectively to extract, vibrate 10 minutes, centrifugal 5 minutes, centrifugally use 1mL pipettor Aspirate supernatant 1mL respectively afterwards, 10mL mobile phase is added respectively with bottleneck pipettor, get 1.5mL after shaken well and fill auto injection bottle, namely sample solution is obtained.It is 47.89wt% that the present embodiment finally obtains Cathinone content in sample one, and in sample two, the content of 4-methyl methcathinone is 48.12wt%.
Checking example 1
(1) select 2-phenyl ethylamine as the process of internal standard compound matter.
Compound concentration is respectively the Cathinone of 0.1mg/mL and the interior mark 2-phenyl ethylamine solution of 0.1mg/mL, Cathinone and interiorly indicate good degree of separation;
Compound concentration is respectively the 4-methyl methcathinone of 0.1mg/mL and the interior mark 2-phenyl ethylamine solution of 0.1mg/mL, 4-methyl methcathinone and interiorly indicate good degree of separation.
(2) foundation of Internal standard working curve method
Experimental technique: get Cathinone Standard Stock solutions, with the inner mark solution that mass concentration is 0.1mg/mL be diluted to successively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the series standard solution of 0.0005mg/mL, and keep the concentration of inner mark solution to be 0.01mg/mL.Get the titer 5 μ L sample introduction of variable concentrations respectively, the peak area of recording responses.Each concentration sample introduction 3 times, and linear regression is carried out to the mean value A of 3 peak area ratios and mass concentration ratio c (mg/mL).
Get 4-methyl methcathinone Standard Stock solutions, with the inner mark solution that mass concentration is 0.1mg/mL be diluted to successively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the series standard solution of 0.0005mg/mL, and keep the concentration of inner mark solution to be 0.01mg/mL.Get the titer 5 μ L sample introduction of variable concentrations respectively, the peak area of recording responses.Each concentration sample introduction 3 times, and linear regression is carried out to the mean value A of 3 peak area ratios and mass concentration ratio c (mg/mL).
Experimental result shows, the range of linearity of Cathinone is 0.005-0.5mg/mL, and linear equation is A=0.8253c-0.3681, R
2=0.9997; The range of linearity of 4-methyl methcathinone is 0.005-0.5mg/mL, and linear equation is A=1.1121c-0.2635, R
2=0.9997.
Checking example 2
The foundation of external standard working curve
Experimental technique: get Cathinone Standard Stock solutions, be diluted to successively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the series standard solution of 0.0005mg/mL.Get the titer 5 μ L sample introduction of variable concentrations respectively, the peak area of recording responses.Each concentration sample introduction 3 times, and linear regression is carried out to the mean value A of 3 peak areas and mass concentration c (mg/mL).
Get 4-methyl methcathinone Standard Stock solutions, be diluted to successively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the series standard solution of 0.0005mg/mL.Get the titer 5 μ L sample introduction of variable concentrations respectively, the peak area of recording responses.Each concentration sample introduction 3 times, and linear regression is carried out to the mean value A of 3 peak areas and mass concentration c (mg/mL).
Experimental result shows, the range of linearity of Cathinone is 0.005-0.5mg/mL, and linear equation is A=6 × 10
6c-13368, R
2=0.9999, detect and be limited to 0.2 μ g/mL (S/N>=3); The range of linearity of 4-methyl methcathinone is 0.005-0.5mg/mL, and linear equation is A=1 × 10
7c+24487, R
2=0.9999, detect and be limited to 0.2 μ g/mL (S/N>=3).
Checking example 3
Precision is investigated
Get the Cathinone of basic, normal, high 3 concentration, 4-methyl methcathinone sample, analyze by the external standard method set up.Extraction and analysis 10 times in 1 day, calculates the in a few days relative standard deviation (RSD) of sample; Continuous 5 days, calculate the relative standard deviation in the daytime of sample, the results are shown in Table 1,2.
The Precision test result of table 1. variable concentrations Cathinone sample
The Precision test result of table 2. variable concentrations 4-methyl methcathinone sample
Comparative example
In investigation prior art, acid modification agent is on the impact of experimental result
(1) phosphoric acid is investigated on the impact of experimental result
Mobile phase: A-0.5% phosphate aqueous solution; B-acetonitrile.
Conclusion: do mobile phase with phosphoric acid, along with organic phase ratio reduces, hangover is serious, and ephedrine is got bad.
(2) trifluoroacetic acid is investigated on the impact of experimental result
Mobile phase: the aqueous solution of A-trifluoroacetic acid (pH=3.5); B-acetonitrile.
Conclusion: do mobile phase by the aqueous solution of trifluoroacetic acid (pH=3.5), obtain good peak shape during low flow velocity, but theoretical cam curve is lower; Become bimodal during high flow rate, and being separated of Cathinone and 4-methyl methcathinone cannot be realized.
Visible, existing acid modification agent cannot meet high flow rate, high theoretical cam curve, testing requirement that peak shape is good.
Above-described embodiment is only for the invention example is clearly described, and the restriction not to the invention embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All within the spirit and principles in the present invention any apparent change of extending out or variation be still among the protection domain of the invention claim.
Claims (10)
1. adopt a method for Cathinone and 4-methyl methcathinone content in liquid chromatography quantitative analysis sample, it comprises the steps:
(1) preparation of working fluid;
(2) preparation of sample solution;
(3) setting of testing conditions;
(4) mensuration of Cathinone and 4-methyl methcathinone sample size;
(5) experimental result calculates,
Wherein, in step (3), chromatographic column adopts anti-phase phenyl chromatographic column, and mobile phase is A-1 ~ 5mM ammonium acetate buffer: B-acetonitrile and/or methyl alcohol, A:B=(20 ~ 40): (60-80), and flow velocity is 1.0-1.5mL/min.
2. method according to claim 1, is characterized in that: in step (3), the 4mM ammonium acetate buffer of A-pH=5.0: B-acetonitrile, A:B=20:80, and flow velocity is 1.2mL/min.
3. method according to claim 1, is characterized in that: adopt inner mark method ration, selects 2-phenyl ethylamine as internal standard compound matter.
4. method according to claim 3, it is characterized in that: in step (1), get Cathinone and 4-methyl methcathinone Standard Stock solutions respectively, by mass concentration be respectively the solution of the internal standard compound matter of 0.1mg/mL be diluted to successively Cathinone and 4-methyl methcathinone mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, two series standard solution of 0.0005mg/mL, and keep the concentration of inner mark solution to be 0.01mg/mL.
5. method according to claim 3, is characterized in that: in step (2): take sample, adds mobile phase and dissolves, vibration, centrifugal, get supernatant after centrifugal, add internal standard compound matter, and add mobile phase, after shaken well, namely obtain sample solution; Mobile phase is identical with the mobile phase in step (3).
6. method according to claim 1, it is characterized in that: adopt quantified by external standard method, wherein, in step (1), get Cathinone, 4-methyl methcathinone Standard Stock solutions respectively, be diluted to successively respectively mass concentration be respectively 0.5,0.1,0.05,0.01,0.005,0.001, the two series standard solution of 0.0005mg/mL.
7. method according to claim 6, is characterized in that: in step (2): take sample, adds mobile phase and dissolves, vibration, centrifugal, gets supernatant, adds mobile phase, namely obtain sample solution after shaken well after centrifugal; Mobile phase is identical with the mobile phase in step (3).
8. the method according to claim 1 to 7 any one, is characterized in that: in step (3), and chromatographic column specification is 250mm × 4.6mm, 5 μm, and column temperature is 35 DEG C, determined wavelength 254nm.
9. the method according to claim 1 to 7 any one, is characterized in that, mobile phase puts into the ultrasonic 10 ~ 15min of ultrasonic cleaner before using after 0.45 μm of micro porous filtration membrane filtration, fully deviates from the gas in mobile phase.
10. the method according to claim 5 or 7 any one, it is characterized in that, before add mobile phase in sample, use the Cathinone in the mixed solution extraction sample of toluene, methyl phenyl ethers anisole, methylene chloride and ether or 4-methyl methcathinone, the volume ratio of toluene, methyl phenyl ethers anisole, methylene chloride and ether is 6:3:2:1.5, in isolated organic phase, add the hydrochloric acid that HCl massfraction is 20%, after removing organic phase residue is placed in 35 DEG C of rapid concentration instrument are concentrated into dry.
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| CN110346470A (en) * | 2019-07-04 | 2019-10-18 | 公安部物证鉴定中心 | A kind of detection method of 3,4- methylene-dioxy methcathinone |
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| CN110146459A (en) * | 2019-06-11 | 2019-08-20 | 公安部物证鉴定中心 | The ftir analysis method of methcathinone in sample |
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