CN115047109A - Method for detecting fentanyl new psychoactive substances in food - Google Patents
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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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- 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
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Abstract
The invention relates to the technical field of food safety detection, and provides a method for detecting fentanyl new psychoactive substances in food, which comprises the following steps: (1) pretreating a sample to be detected to obtain a sample solution to be loaded on a machine; (2) drawing a standard curve of fentanyl, remifentanil, sufentanil, alfentanil, acefentanil; (3) and (3) carrying out HPLC-MS/MS detection on the to-be-detected sample solution, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentrations of the 7 components in the to-be-detected sample. The detection method can accurately and efficiently identify whether the fentanyl psychoactive substances exist in the food or not, and can specifically distinguish various fentanyl analogs and isomers thereof. Compared with the traditional method, the method has the advantages of simple and quick operation, high recovery rate, low detection limit and reduction of the requirements of operators.
Description
Technical Field
The invention relates to the technical field of food safety detection, in particular to a method for detecting fentanyl new psychoactive substances in food.
Background
Fentanyl (fentanyl) is a synthetic opioid, first synthesized by Paul Janseen, scientist Belgium in 1960, sold as an analgesic with pharmacological effects similar to morphine, which is 80 times as potent as morphine. Fentanyl drugs are the major narcotic drugs in the clinic, but once overdosed, they can lead to the risk of respiratory depression and even death. Because fentanyl has a powerful analgesic effect, can interact with central specific receptors, relieve pain and produce a euphoric (happiness) feeling substance, if the special controlled drug substances comply with relevant regulations of drug administration, the drugs are reasonably prepared and used, and the drugs can be used for treating diseases and treating the diseases according to the recommended application and dosage of the orders and become well-known drugs once being abused. The fentanyl new psychotropic active substance has strong drug effect, high lethality and serious abuse, the fentanyl substance is widely used, and the phenomena of non-medicinal use and abuse of the fentanyl also occur. 6 fentanyl, remifentanil, sufentanil and carfentanil are common, and novel fentanyl analogs are continuously appearing (more than 60 reports are available at present). At present, the problems of manufacturing, smuggling and abuse of fentanyl substances are more and more prominent in the global scope, and the fentanyl new psychoactive substances have the characteristics of strong toxicity, quick change, multiple varieties, difficult investigation and the like, so that great challenges are provided for detection and inspection work. Corresponding laws and regulations are made for the control of various countries in order to ensure normal public order and national security.
Fentanyl (and its derivatives) bind to opioid μ receptors and have high affinity, high lipid solubility and strong intrinsic activity. The fentanyl is not only an important pharmacological and pharmacodynamic action characteristic of fentanyl, but also a main reason for causing fatal adverse reaction or toxicity of the fentanyl, and has the advantages of strong analgesic effect and high abuse potential, can quickly penetrate through cell membranes and enter the brain through a blood brain barrier, forms a blood-medicine peak in a short time, and is very easy to form tolerance and drug dependence. Fentanyl is absorbed through the skin, mucous membranes and, therefore, such substance poisoning occurs not only in abusers, but also in workers who are handled or contacted by fentanyl-type drugs without protective measures. However, at present, the prevention of the abuse of fentanyl new psychoactive substances, the attack of drug taking, drug selling and drug smuggling are only limited to the detection of the content of biological matrixes (such as blood, urine, hair and the like), and the detection is all followed by monitoring and verification.
The assays suitable for the initial screening of fentanyl and derivatives thereof in biological samples vary, for example: immunoassay, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry (HPLC-MS/MS) methods, and the like. Immunoassays are one method of making assays that utilize specific binding of an antigen (target) and an antibody, but different immunoassays have limitations on the cross-reactivity of fentanyl analogs, and some cross-reactivity is unknown; the gas chromatography-mass spectrometry method cannot directly measure non-volatile, polar or thermally unstable substances, requires derivatization reaction on a target substance, and is inconsistent with the development trend of rapid and efficient analytical chemistry in the future. Compared with a gas chromatography-mass spectrometry method, the liquid chromatography-mass spectrometry method is higher in sensitivity, more stable and wider in application range, but the liquid chromatography-mass spectrometry detection method of fentanyl substances in food is less in report at present, so that the illegal phenomenon that the fentanyl substances permeate into the food occurs. At present, the fentanyl psychoactive substances in food have no national authoritative detection standard, and the existing visible detection method only comprises the detection method research of the fentanyl psychoactive substances in a biological matrix, and is post-incident monitoring and verification for preventing abuse of the fentanyl psychoactive substances. However, the biological sample has complex components and numerous interferents, which brings certain difficulty to qualitative and quantitative analysis of fentanyl, the pretreatment process of detection of the fentanyl substance in the biological matrix sample is complicated and time-consuming, a large amount of organic solvent is needed, potential safety hazards exist, and the environment is polluted; the concentration content of fentanyl drugs in the biological matrix is generally low, so that the requirement on the detection sensitivity of fentanyl is high, a single detection method cannot meet the requirement, multiple instrument comprehensive analysis and various combination techniques are generally adopted for analysis, and the related detection method for detecting fentanyl by using the biological matrix sample is not suitable for the food matrix. The method is used for developing research for identifying the fentanyl psychoactive substances in the food, carrying out post-monitoring and verification on the abuse prevention of the fentanyl psychoactive substances, advancing the prevention and source control to the front end, and establishing a method with convenient and quick pretreatment, sensitive detection and accurate quantification to measure the residual quantity of the fentanyl psychoactive substance components in the food so as to accurately identify whether the fentanyl psychoactive substances are contained in the food. The fentanyl substance monitoring system is quite necessary for maintaining the health of the vast people and guaranteeing the food safety on the tongue tip, provides powerful technical support for case law enforcement, and can monitor key suspected persons and persons engaged in special industries by public security agencies, monitor the abuse condition and the prevalence trend of fentanyl substances, prevent social events from happening, and realize accurate, rapid and real-time monitoring on fentanyl mental active substances. Therefore, a reliable, rapid and accurate analytical detection method for identifying fentanyl substances in food is needed and applied to solving the practical problems. The aspects of preventing fentanyl abuse, fighting drug taking and drug vending and drug smuggling are transferred from post-monitoring verification to pre- (front-end) prevention and source control.
Disclosure of Invention
The invention aims to provide a method for detecting fentanyl type new psychoactive substances in food, which can accurately and efficiently identify whether the fentanyl type psychoactive substances exist in the food, and can specifically distinguish various fentanyl analogs and isomers thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for detecting fentanyl new psychotropic active substances in food, which comprises the following steps:
(1) mixing a sample to be detected, water and acetonitrile, then sequentially mixing with anhydrous sodium acetate powder and anhydrous magnesium sulfate, centrifuging, taking supernatant, performing rotary evaporation, eluting and filtering to obtain a sample solution to be processed;
(2) preparing a series of standard solutions of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil with gradually increased concentrations, sequentially carrying out HPLC-MS/MS detection on the standard solutions, and drawing a standard curve of the 7 components;
(3) and (3) carrying out HPLC-MS/MS detection on the to-be-detected sample solution, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentrations of the 7 components in the to-be-detected sample.
Further, in the step (1), the dosage ratio of the sample to be detected, water, acetonitrile, anhydrous sodium acetate powder and anhydrous magnesium sulfate is 1.80-2.20 g, 2-5 mL, 12-18 mL, 1.4-1.6 g and 5-8 g.
Further, the rotating speed of the centrifugation in the step (1) is 3500-4500 r/min, and the time of the centrifugation is 3-8 min.
Further, the rotary evaporation temperature in the step (1) is 40-50 ℃, and the rotary evaporation is finished until no liquid exists in the sample.
Further, the eluent eluted in the step (1) comprises aqueous formic acid solution containing ammonium acetate and acetonitrile; the ratio of the ammonium acetate-containing formic acid aqueous solution to acetonitrile is 8-12: 1, the concentration of ammonium acetate in the ammonium acetate-containing formic acid aqueous solution is 3-8 mmol/L, and the content of formic acid in the ammonium acetate-containing formic acid aqueous solution is 0.08% -0.12%.
Further, in the step (1), filtration was performed using a 0.22 μm nylon 66 organic filter.
Further, the sample to be detected in the step (1) is solid food or liquid food.
Further, the chromatographic conditions of HPLC-MS/MS detection in the step (3) are as follows: adopting a Waters ACQUITY UPLClM BHE C18 chromatographic column, wherein the sample injection amount is 4-6 mu L, the chromatographic column temperature is 34-36 ℃, and the flow of a mobile phase is 0.2-0.4 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-1.0 min, 10% of mobile phase B; 1.1-3.0 min, 65% of mobile phase B; 3.1-4.0 min, 65% of mobile phase B; 4.1-6.0 min, 10% of mobile phase B.
Further, the chromatographic conditions of HPLC-MS/MS detection in the step (3) are as follows: adopting an ACQUITY UPLC @ HSST3 chromatographic column, wherein the sample injection amount is 4-6 mu L, the chromatographic column temperature is 34-36 ℃, and the flow of a mobile phase is 0.2-0.4 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-0.5 min, 10% of mobile phase B; 0.5-1.0 min, 35% of mobile phase B; 1.0-2.5 min, 35% of mobile phase B; 2.5-3.5 min, 35-10% of mobile phase B; 3.5-6.0 min, 10% of mobile phase B.
Further, mass spectrum conditions of HPLC-MS/MS detection in the step (3) are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5000-6000V;
ion source temperature: 500-600 ℃;
air pressure of an air curtain: 24-26 psi;
collision air pressure: 8-12 psi;
spraying air pressure: 54-56 psi;
heating the air pressure: 54-56 psi;
an acquisition mode: multiple reaction monitoring mode MRM.
Compared with the prior art, the invention has the beneficial effects that:
the invention overcomes key technologies such as complex food matrix sample treatment, high-accuracy identification and quantification and establishes a rapid, accurate and efficient method for detecting multiple fentanyl in food through series of tests, thereby identifying whether the fentanyl psychoactive substances exist in the food, monitoring and verifying the prevention of abuse of the fentanyl psychoactive substances after engaging in, and advancing the prevention and source control to the front end. The invention not only is necessary for maintaining the health of the vast people and guaranteeing the food safety on the tongue tip, but also provides powerful technical support for case law enforcement, and simultaneously can monitor key suspected people and special industry professional people for the fentanyl substance in public security institutions, monitor the abuse condition and the prevalence trend of the fentanyl substance, prevent the occurrence of social hazards and realize accurate, rapid and real-time monitoring on the fentanyl mental active substance. Fentanyl class because of the continuous update of the 'fentanyl family', a plurality of analogues or structural isomers with similar structures appear, and the detection method has high resolution and high specificity to distinguish various fentanyl analogues and isomers thereof. Compared with the traditional method, the method has the advantages of simple and quick operation, high recovery rate, low detection limit and reduction of the requirements of operators.
Drawings
FIG. 1 is a detection spectrum of cola as a detection sample in example 5;
FIG. 2 is a detection map of 7 fentanyl standards.
Detailed Description
The invention provides a method for detecting fentanyl new psychoactive substances in food, which comprises the following steps:
(1) mixing a sample to be detected, water and acetonitrile, then sequentially mixing with anhydrous sodium acetate powder and anhydrous magnesium sulfate, centrifuging, taking supernatant, performing rotary evaporation, eluting and filtering to obtain a sample solution to be processed;
(2) preparing a series of standard solutions of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil with gradually increased concentrations, sequentially carrying out HPLC-MS/MS detection on the standard solutions, and drawing a standard curve of the 7 components;
(3) and (3) carrying out HPLC-MS/MS detection on the to-be-detected sample solution, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentrations of the 7 components in the to-be-detected sample.
Mixing a sample to be detected, water and acetonitrile, then sequentially mixing the mixture with anhydrous sodium acetate powder and anhydrous magnesium sulfate, centrifuging, taking supernatant, carrying out rotary evaporation, eluting and filtering to obtain a sample solution to be detected; the using ratio of the sample to be detected, water, acetonitrile, anhydrous sodium acetate powder and anhydrous magnesium sulfate is 1.80-2.20 g: 2-5 mL: 12-18 mL: 1.4-1.6 g: 5-8 g, the preferred is that the sample to be detected, water, acetonitrile, anhydrous sodium acetate powder and anhydrous magnesium sulfate are 1.90-2.10 g: 3-4 mL: 14-16 mL: 1.45-1.55 g: 6-7 g, and the further preferred is that the sample to be detected, water, acetonitrile, anhydrous sodium acetate powder and anhydrous magnesium sulfate are 1.95-2.05 g: 3.3-3.7 mL: 14.5-15.5 mL: 1.48-1.52 g: 6.2-6.8 g.
In the invention, the rotation speed of the centrifugation is 3500-4500 r/min, preferably 3600-4300 r/min, and more preferably 3800-4200 r/min; the centrifugation time is 3-8 min, preferably 4-7 min, and further preferably 5-6 min; the centrifugation was performed using an Allegra 64R refrigerated bench-top high speed centrifuge (Beckman Coulter, USA).
In the invention, the temperature of the rotary evaporation is 40-50 ℃, preferably 42-48 ℃, and further preferably 44-46 ℃; the time of the rotary evaporation is preferably until no liquid in the sample is finished.
In the present invention, the eluted eluent comprises an aqueous formic acid solution containing ammonium acetate and acetonitrile; the ratio of the ammonium acetate-containing formic acid aqueous solution to acetonitrile is 8-12: 1, preferably 9-11: 1, and more preferably 9.5-10.5: 1; the concentration of ammonium acetate in the ammonium acetate-containing formic acid aqueous solution is 3-8 mmol/L, preferably 4-7 mmol/L, and further preferably 5-6 mmol/L; the content of formic acid in the aqueous solution of formic acid containing ammonium acetate is 0.08-0.12%, preferably 0.09-0.11%, and more preferably 0.10%.
In the present invention, the filtration is preferably performed using a 0.22 μm nylon 66 organic filter.
In the present invention, the sample to be detected is preferably a solid food or a liquid food.
In the invention, a series of standard solutions of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil with increasing concentrations are prepared, HPLC-MS/MS detection is sequentially carried out on the standard solutions, and a standard curve of the 7 components is drawn.
In the invention, HPLC-MS/MS detection is carried out on the to-be-detected sample solution, and the response values of all components are substituted into the standard curve obtained in the step (2) to obtain the concentrations of the 7 components in the to-be-detected sample.
In the invention, the chromatographic conditions of the HPLC-MS/MS detection are as follows: using a Waters acquityuppllcm BHE C18 chromatography column; the sample injection amount is 4-6 muL, preferably 4.5-5.5 muL, and more preferably 4.8-5.2 muL; the temperature of the chromatographic column is 34-36 ℃, preferably 34.5-35.5 ℃, and more preferably 34.8-35.2 ℃; the flow rate of the mobile phase is 0.2-0.4 mL/min, preferably 0.25-0.35 mL/min, and more preferably 0.28-0.32 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-1.0 min, 10% of mobile phase B; 1.1-3.0 min, 65% of mobile phase B; 3.1-4.0 min, 65% of mobile phase B; 4.1-6.0 min, 10% of mobile phase B.
In the invention, the chromatographic conditions of the HPLC-MS/MS detection are as follows: an ACQUITY UPLC @ HSST3 chromatographic column is adopted, the sample injection amount is 4-6 mu L, preferably 4.5-5.5 mu L, and further preferably 4.8-5.2 mu L; the temperature of the chromatographic column is 34-36 ℃, preferably 34.5-35.5 ℃, and more preferably 34.8-35.2 ℃; the flow rate of the mobile phase is 0.2-0.4 mL/min, preferably 0.25-0.35 mL/min, and more preferably 0.28-0.32 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-0.5 min, 10% of mobile phase B; 0.5-1.0 min, 35% of mobile phase B; 1.0-2.5 min, 35% of mobile phase B; 2.5-3.5 min, 35-10% of mobile phase B; 3.5-6.0 min, 10% of mobile phase B.
In the invention, the mass spectrum conditions of the HPLC-MS/MS detection are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5000-6000V, preferably 5200-5800V, and more preferably 5400-5600V;
ion source temperature: 500-600 ℃, preferably 520-580 ℃, and more preferably 540-560 ℃;
air pressure of an air curtain: 24-26 psi, preferably 25 psi;
collision air pressure: 8-12 psi, preferably 9-11 psi, and more preferably 10 psi;
spraying air pressure: 54-56 psi, preferably 55 psi;
heating the air pressure: 54-56 psi, preferably 55 psi;
an acquisition mode: multiple reaction monitoring mode MRM.
In the invention, the mass spectrometer for HPLC-MS/MS detection is an AB3500 triple quadrupole mass spectrometer (ABSCIEX company, USA), and the chromatograph is an Shimadzu ultra-high performance liquid chromatograph.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a method for detecting fentanyl type new psychoactive substances in bread, which comprises the following steps:
(1) 2.00g of bread (to which 0.100mL of each of fentanyl, sufentanil, remifentanil, alfentanil, acetylfentanyl, and carfentanil at a concentration of 400ng/mL were added) was weighed, 3.5mL of water and 15mL of acetonitrile (analytical grade) were added, and after vortex mixing for 1min, adding mixed powder of 1.5g anhydrous sodium acetate, rapidly shaking, mixing with vortex for 1min, adding 6g anhydrous magnesium sulfate, rapidly shaking, continuously mixing with vortex (2300r/min) for 5min, centrifuging at 4000r/min for 5min, transferring all supernatant into a heart-shaped bottle, spin-evaporating at 45 deg.C to dry, eluting with 2mL eluent (0.1% formic acid water solution containing 5mmol/L ammonium acetate: acetonitrile (chromatographic grade): 9:1), and filtering with 0.22 μm nylon 66 organic filter membrane to obtain the sample solution to be loaded onto the machine;
(2) preparing a standard stock solution: accurately weighing 10mg (accurate to 0.01mg) of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil standard substances respectively into a small beaker, adding 0.1% methanoic acid solution for dissolving, quantitatively transferring the solution into a 10mL volumetric flask, diluting the solution to a scale by using 0.1% methanoic acid solution, shaking uniformly, and preparing into standard stock solutions with the concentrations of 1.0 mg/mL;
preparation of mixed standard intermediate solution 1: accurately sucking 100 mu L of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil mixed standard stock solutions with the concentration of 1.0mg/mL into the same 100mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 1 containing 1.0 mu g/mL of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil;
preparing a mixed standard intermediate solution 2: accurately sucking 1.0mL of the mixed standard intermediate solution into a 10mL volumetric flask, performing constant volume to scale with acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 2 containing fentanyl, remifentanil, sufentanil, alfentanil and acetylfentanyl with the concentration of 0.10 mu g/mL;
preparation of standard working solution: accurately sucking 200 mul, 400 mul and 1000 mul of the mixed standard intermediate solution 2 and the mixed standard intermediate solution 1 respectively into a 20mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and uniformly shaking to obtain a series of standard working solutions with the concentrations of fentanyl, remifentanil, sufentanil, alfentanil, carfentanil and alfentanil of 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL and 50.0 ng/mL;
sequentially carrying out HPLC-MS/MS detection on the obtained series of standard working solutions, and drawing a standard curve of each solution by taking the concentration of each solution as an abscissa and the response value obtained by the determination as an ordinate;
(3) carrying out HPLC-MS/MS detection on the sample solution to be tested, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentration of the 7 components in the sample to be tested;
the chromatographic conditions of HPLC-MS/MS detection are as follows: adopting a Waters ACQUITY UPLClM BHE C18 chromatographic column, wherein the sample injection amount is 5 μ L, the chromatographic column temperature is 35 ℃, and the mobile phase flow is 0.3 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-1.0 min, 10% of mobile phase B; 1.1-3.0 min, 65% of mobile phase B; 3.1-4.0 min, 65% of mobile phase B; 4.1-6.0 min, 10% of mobile phase B;
the mass spectrum conditions of HPLC-MS/MS detection are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5500V;
ion source temperature: 550 ℃;
air pressure of an air curtain: 25 psi;
collision air pressure: 9 psi;
spraying air pressure: 55 psi;
heating the air pressure: 55 psi;
an acquisition mode: a multiple reaction monitoring mode, MRM;
the mass spectral parameters of each compound are shown in table 1:
table 1: mass Spectrometry parameters of the Compounds
Note: as quantitative ion pairs
Example 2
The embodiment provides a method for detecting fentanyl new psychoactive substances in pastries, which comprises the following steps:
(1) 2.00g of confectionery (wherein 0.100mL each of fentanyl, sufentanil, remifentanil, alfentanil, acetylfentanil, carfentanil and alfentanil at a concentration of 400ng/mL were added), 3.0mL of water and 14mL of acetonitrile (analytical grade) were added, and after vortex mixing for 1min, adding mixed powder of 1.55g anhydrous sodium acetate, rapidly shaking, mixing with vortex for 1min, adding 7g anhydrous magnesium sulfate, rapidly shaking, continuously mixing with vortex (2300r/min) for 5min, centrifuging at 3500r/min for 6min, transferring all supernatant into a chicken heart bottle, spin-evaporating at 50 deg.C to dry, eluting with 2mL eluent (composed of 5mmol/L ammonium acetate in 0.1% formic acid water solution: acetonitrile (chromatographic grade): 8:1), and filtering with 0.22 μm nylon 66 organic filter membrane to obtain the sample solution to be loaded onto the machine;
(2) preparing a standard stock solution: accurately weighing 10mg (accurate to 0.01mg) of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil standard substances respectively into a small beaker, adding 0.1% methanoic acid solution for dissolving, quantitatively transferring the solution into a 10mL volumetric flask, diluting the solution to a scale by using 0.1% methanoic acid solution, shaking uniformly, and preparing into standard stock solutions with the concentrations of 1.0 mg/mL;
preparation of mixed standard intermediate solution 1: accurately sucking 100 mu L of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil mixed standard stock solutions with the concentration of 1.0mg/mL into the same 100mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 1 containing 1.0 mu g/mL of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil;
preparing a mixed standard intermediate solution 2: accurately sucking 1.0mL of the mixed standard intermediate solution into a 10mL volumetric flask, performing constant volume to scale with acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 2 containing fentanyl, remifentanil, sufentanil, alfentanil and acetylfentanyl with the concentration of 0.10 mu g/mL;
preparation of standard working solution: accurately sucking 200 mul, 400 mul and 1000 mul of the mixed standard intermediate solution 2 and the mixed standard intermediate solution 1 respectively into a 20mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and uniformly shaking to obtain a series of standard working solutions with the concentrations of fentanyl, remifentanil, sufentanil, alfentanil, carfentanil and alfentanil of 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL and 50.0 ng/mL;
sequentially carrying out HPLC-MS/MS detection on the obtained series of standard working solutions, taking the concentration of each solution as a horizontal coordinate, taking the response value obtained by the detection as a vertical coordinate, and drawing a standard curve of each solution;
(3) carrying out HPLC-MS/MS detection on the sample solution to be tested, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentration of the 7 components in the sample to be tested;
the chromatographic conditions of HPLC-MS/MS detection are as follows: adopting a Waters ACQUITY UPLClM BHE C18 chromatographic column, wherein the sample injection amount is 5 μ L, the chromatographic column temperature is 36 ℃, and the mobile phase flow is 0.4 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-1.0 min, 10% of mobile phase B; 1.1-3.0 min, 65% of mobile phase B; 3.1-4.0 min, 65% of mobile phase B; 4.1-6.0 min, 10% of mobile phase B;
the mass spectrum conditions of HPLC-MS/MS detection are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5600V;
ion source temperature: 540 ℃;
air curtain pressure: 25 psi;
collision air pressure: 10 psi;
spraying air pressure: 55 psi;
heating the air pressure: 55 psi;
an acquisition mode: multiple reaction monitoring mode MRM;
the mass spectral parameters of each compound are shown in table 1.
Example 3
The embodiment provides a method for detecting fentanyl type new psychoactive substances in milk powder, which comprises the following steps:
(1) 2.10g of milk powder (to which 0.100mL each of fentanyl, sufentanil, remifentanil, alfentanil, acetylfentanyl, and alfentanil at a concentration of 400ng/mL were added, at a concentration of 400 ng/mL) was weighed, 4.0mL of water and 16mL of acetonitrile (analytical grade) were added, and after vortex mixing was performed for 1min, adding mixed powder of 1.45g anhydrous sodium acetate, rapidly shaking, mixing with vortex for 1min, adding 6.5g anhydrous magnesium sulfate, rapidly shaking, continuously mixing with vortex (2300r/min) for 5min, centrifuging at 4500r/min for 4min, transferring all supernatant into a heart-shaped bottle, spin-evaporating at 40 deg.C to dry, eluting with 2mL eluent (0.1% formic acid water solution containing 5mmol/L ammonium acetate: acetonitrile (chromatographic grade): 10:1), and filtering with 0.22 μm nylon 66 organic filter membrane to obtain the sample solution to be loaded onto the machine;
(2) preparing a standard stock solution: accurately weighing 10mg (accurate to 0.01mg) of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil standard substances respectively into a small beaker, adding 0.1% methanoic acid solution for dissolving, quantitatively transferring the solution into a 10mL volumetric flask, diluting the solution to a scale by using 0.1% methanoic acid solution, shaking uniformly, and preparing into standard stock solutions with the concentrations of 1.0 mg/mL;
preparation of mixed standard intermediate solution 1: accurately sucking 100 mu L of fentanyl, remifentanil, sufentanil, alfentanil, carfentanil, alfentanil and acetylfentanil mixed standard stock solutions with the concentration of 1.0mg/mL into the same 100mL volumetric flask, fixing the volume to the scale by using acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 1 containing 1.0 mu g/mL of fentanyl, remifentanil, sufentanil, oxfentanil, carfentanil, alfentanil and acetylfentanil;
preparing a mixed standard intermediate solution 2: accurately sucking 1.0mL of the mixed standard intermediate solution into a 10mL volumetric flask, performing constant volume to scale with acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 2 containing fentanyl, remifentanil, sufentanil, alfentanil and acetylfentanyl with the concentration of 0.10 mu g/mL;
preparation of standard working solution: accurately sucking 200 mu L, 400 mu L and 1000 mu L of the mixed standard intermediate solution 2 and the mixed standard intermediate solution 1 respectively into a 20mL volumetric flask, fixing the volume to scale by acetonitrile (chromatographic grade), and shaking uniformly to obtain a series of standard working solutions with the concentrations of fentanyl, remifentanil, sufentanil, oxfentanil, carfentanil, alfentanil and acetylfentanyl of 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL and 50.0 ng/mL;
sequentially carrying out HPLC-MS/MS detection on the obtained series of standard working solutions, and drawing a standard curve of each solution by taking the concentration of each solution as an abscissa and the response value obtained by the determination as an ordinate;
(3) carrying out HPLC-MS/MS detection on the sample solution to be tested, and substituting the response values of all the components into the standard curve obtained in the step (2) to obtain the concentrations of the 7 components in the sample to be tested;
the chromatographic conditions of HPLC-MS/MS detection are as follows: adopting ACQUITY UPLC @ HSST3 chromatographic column, wherein the sample volume is 5 μ L, the temperature of the chromatographic column is 34 ℃, and the flow rate of the mobile phase is 0.3 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-0.5 min, 10% B; 0.5-1.0 min, 35% B; 1.0-2.5 min, 35% B; 2.5-3.5 min, 35-10% of B; 3.5-6.0 min, 10% of B;
the mass spectrum conditions of HPLC-MS/MS detection are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5400V;
ion source temperature: 560 ℃;
air pressure of an air curtain: 25 psi;
collision air pressure: 10 psi;
spraying air pressure: 55 psi;
heating the air pressure: 55 psi;
an acquisition mode: multiple reaction monitoring mode MRM;
the mass spectral parameters of each compound are shown in table 1.
Example 4
The embodiment provides a method for detecting fentanyl type new psychoactive substances in milk, which comprises the following steps:
(1) 2.00g of milk (to which 0.100mL each of fentanyl, sufentanil, remifentanil, alfentanil, acetylfentanyl, carfentanil and alfentanil at a concentration of 400ng/mL were added) was weighed, 2.5mL of water and 16mL of acetonitrile (analytical grade) were added, and after vortex mixing for 1min, adding mixed powder of 1.4g anhydrous sodium acetate, rapidly shaking, mixing with vortex for 1min, adding 7g anhydrous magnesium sulfate, rapidly shaking, continuously mixing with vortex (2300r/min) for 5min, centrifuging at 4000r/min for 5min, transferring all supernatant into a heart-shaped bottle, spin-evaporating at 48 deg.C to dry, eluting with 2mL eluent (containing 5mmol/L ammonium acetate in 0.1% formic acid water solution: acetonitrile (chromatographic grade): 9:1), and filtering with 0.22 μm nylon 66 organic filter membrane to obtain the sample solution to be loaded into the machine;
(2) preparing a standard stock solution: accurately weighing 10mg (accurate to 0.01mg) of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil standard substances respectively into a small beaker, adding 0.1% methanoic acid solution for dissolving, quantitatively transferring the solution into a 10mL volumetric flask, diluting the solution to a scale by using 0.1% methanoic acid solution, shaking uniformly, and preparing into standard stock solutions with the concentrations of 1.0 mg/mL;
preparation of mixed standard intermediate solution 1: accurately sucking 100 mu L of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil mixed standard stock solutions with the concentration of 1.0mg/mL into the same 100mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 1 containing 1.0 mu g/mL of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil;
preparing a mixed standard intermediate solution 2: accurately sucking 1.0mL of the mixed standard intermediate solution into a 10mL volumetric flask, performing constant volume to scale with acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 2 containing fentanyl, remifentanil, sufentanil, alfentanil and acetylfentanyl with the concentration of 0.10 mu g/mL;
preparation of standard working solution: accurately sucking 200 mul, 400 mul and 1000 mul of the mixed standard intermediate solution 2 and the mixed standard intermediate solution 1 respectively into a 20mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and uniformly shaking to obtain a series of standard working solutions with the concentrations of fentanyl, remifentanil, sufentanil, alfentanil, carfentanil and alfentanil of 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL and 50.0 ng/mL;
sequentially carrying out HPLC-MS/MS detection on the obtained series of standard working solutions, and drawing a standard curve of each solution by taking the concentration of each solution as an abscissa and the response value obtained by the determination as an ordinate;
(3) carrying out HPLC-MS/MS detection on the sample solution to be tested, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentration of the 7 components in the sample to be tested;
the chromatographic conditions of HPLC-MS/MS detection are as follows: adopting a Waters ACQUITY UPLClM BHE C18 chromatographic column, wherein the sample injection amount is 5 μ L, the chromatographic column temperature is 36 ℃, and the mobile phase flow is 0.3 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-1.0 min, 10% of mobile phase B; 1.1-3.0 min, 65% of mobile phase B; 3.1-4.0 min, 65% of mobile phase B; 4.1-6.0 min, 10% of mobile phase B;
the mass spectrum conditions of HPLC-MS/MS detection are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5500V;
ion source temperature: 550 ℃;
air pressure of an air curtain: 25 psi;
collision air pressure: 9 psi;
spraying air pressure: 55 psi;
heating the air pressure: 55 psi;
an acquisition mode: multiple reaction monitoring mode MRM;
the mass spectral parameters of each compound are shown in table 1.
Example 5
The embodiment provides a method for detecting fentanyl type new psychoactive substances in cola, which comprises the following steps:
(1) weighing 2.10g cola negative sample 2 parts (wherein 1 part is added with fentanyl, sufentanil, remifentanil, alfentanil, acetylfentanyl, carfentanil and alfentanil with concentration of 80ng/mL each 0.100mL), adding 2mL water and 15mL acetonitrile (analytical grade), mixing by vortex for 1min, adding mixed powder of 1.5g anhydrous sodium acetate, quickly shaking, mixing by vortex for 1min, adding 6g anhydrous magnesium sulfate, quickly shaking, mixing by continuous vortex (2300r/min) for 5min, centrifuging by 4500r/min for 4min, transferring all supernatant into a chicken heart bottle, rotary steaming at 40 deg.C to dry, eluting by 2.00mL eluent (0.1% formic acid aqueous solution containing 5mmol/L ammonium acetate: acetonitrile (chromatographic grade) ═ 9:1), passing through a nylon 66 organic filter membrane with 0.22 μm, obtaining a negative sample matrix blank (for a subsequent matrix standard curve) and a to-be-loaded sample (containing a standard substance) solution;
(2) preparing a standard stock solution: accurately weighing 10mg (accurate to 0.01mg) of fentanyl, remifentanil, sufentanil, alfentanil, carfentanil and acetylfentanil standard products respectively into a small beaker, adding 0.1% formic acid methanol solution for dissolving, quantitatively transferring the solution into a 10mL volumetric flask, diluting the solution to a scale by using 0.1% formic acid methanol solution, shaking up, and preparing standard stock solutions with the concentrations of 1.0 mg/mL;
preparation of mixed standard intermediate solution 1: accurately sucking 100 mu L of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil mixed standard stock solutions with the concentration of 1.0mg/mL into the same 100mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 1 containing 1.0 mu g/mL of fentanyl, remifentanil, sufentanil, alfentanil, and acetylfentanil;
preparing a mixed standard intermediate solution 2: accurately sucking 1.0mL of the mixed standard intermediate solution into a 10mL volumetric flask, performing constant volume to scale with acetonitrile (chromatographic grade), and shaking uniformly to obtain a mixed standard intermediate solution 2 containing fentanyl, remifentanil, sufentanil, alfentanil and acetylfentanyl with the concentration of 0.10 mu g/mL;
preparation of standard working solution: accurately sucking 200 mul, 400 mul and 1000 mul of the mixed standard intermediate solution 2 and the mixed standard intermediate solution 1 respectively into a 20mL volumetric flask, performing constant volume to scale by using acetonitrile (chromatographic grade), and uniformly shaking to obtain a series of standard working solutions with the concentrations of fentanyl, remifentanil, sufentanil, alfentanil, carfentanil and alfentanil of 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL and 50.0 ng/mL; in the same way, the negative sample matrix blank prepared in the previous step is used for replacing acetonitrile to prepare a matrix series standard working solution.
Sequentially carrying out HPLC-MS/MS detection on the obtained series of standard working solutions, and drawing a standard curve of each solution by taking the concentration of each solution as an abscissa and the response value obtained by the determination as an ordinate;
(3) carrying out HPLC-MS/MS detection on the sample solution to be tested, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentration of the 7 components in the sample to be tested;
the chromatographic conditions of HPLC-MS/MS detection are as follows: adopting ACQUITY UPLC @ HSST3 chromatographic column, wherein the sample volume is 5 μ L, the temperature of the chromatographic column is 35 ℃, and the flow rate of the mobile phase is 0.3 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-0.5 min, 10% of mobile phase B; 0.5-1.0 min, 35% of mobile phase B; 1.0-2.5 min, 35% of mobile phase B; 2.5-3.5 min, 35-10% of mobile phase B; 3.5-6.0 min, 10% of mobile phase B;
the mass spectrum conditions of HPLC-MS/MS detection are as follows:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5500V;
ion source temperature: 550 ℃;
air pressure of an air curtain: 25 psi;
collision air pressure: 9 psi;
spraying air pressure: 55 psi;
heating the air pressure: 55 psi;
an acquisition mode: multiple reaction monitoring mode MRM;
the mass spectral parameters of each compound are shown in table 1.
Examples of the experiments
The detection and analysis results of the detection methods of examples 1-5 are shown in Table 2, wherein the detection map of example 5 is shown in figure 1, and the maps of 7 fentanyl standard products are shown in figure 2.
Table 2: tables of results of detection and analysis in examples 1 to 5
The linear equation, the matrix standard curve formulation and the matrix effect, detection limit, recovery, precision and accuracy were examined using the assay method of example 5.
Matrix effect: calculating a linear equation of each compound from the 6 points, wherein the lowest concentration is LOQ (S/N is more than or equal to 10), ensuring that the concentration of an actual sample falls within a linear range, and calculating a correlation coefficient (R); after the negative blank similar samples are treated according to the pretreatment method, the final eluent is collected, a standard curve with the concentration range of 1-50 ng/mL is prepared, the matrix effect is investigated at the same time, the slope of the matrix matching standard curve and the standard solution curve is calculated after sample injection analysis, the ratio of the two is taken as the matrix effect, and the result is shown in table 3.
Table 3: results of matrix effect investigation
According to the test, through comparing similar fentanyl with the same concentration, the same fentanyl is respectively prepared by using reagent eluent and negative blank sample eluent, the matrix effect of 7 fentanyl in cola beverage food matrix is not obvious, the matrix effect is between 77.3% and 94.6%, and the matrix inhibition effect is generally shown. However, in order to improve the quantitative accuracy, the external standard method of the matrix matching curve is still suggested for quantification. Part of the matrix effect was counteracted by using the initial mobile phase eluent on the machine for the standard solution profile configuration (see table 4). Different food matrixes have different matrix effects, some inhibition or some enhancement.
Table 4: matrix Effect (%) comparison of different concentrations of fentanyl Material in different food matrices
Detection limit: adding 7 mixed standard solutions with different concentrations into a blank sample, performing pretreatment according to the sample, and performing detection on the sample by using a computer, wherein the mass concentration when the signal-to-noise ratio S/N is greater than or equal to 3 is taken as a detection limit, the mass concentration when the signal-to-noise ratio S/N is greater than or equal to 10 is taken as a quantitative limit, and the quantitative limit is taken as the minimum concentration of a linear range. The detection limit of the 7 fentanyl except alfentanil is 1.0ng/mL (or 1.0ng/mg), the other 6 fentanyl can reach 0.5ng/mL (mg), the quantification limit is 5ng/mL (or 5.0ng/mg), the quantification limit is 0.1ng/mL (or 0.1ng/mg) according to the signal-to-noise ratio alfentanil detection limit can reach 0.05ng/mL (mg), and the results are shown in Table 5.
Table 5: 7 fentanyl signal-to-noise ratios
Recovery, precision and accuracy tests: taking a sample to be loaded into a machine, adding 7 mixed standard solutions with three concentrations of 5.0, 10 and 50ng/mg, pre-treating the sample, loading the sample into the machine for detection, and calculating the recovery rate (accuracy) and precision, wherein the result is shown in Table 6.
Table 6: regression equation, linear range, correlation coefficient, precision and accuracy for each fentanyl
The above examples show that the invention provides a method for detecting fentanyl type psychoactive substances in food, the detection method of the invention can accurately and efficiently identify whether the fentanyl type psychoactive substances exist in the food, and various fentanyl analogs and isomers thereof can be specifically distinguished.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for detecting fentanyl new psychoactive substances in food is characterized by comprising the following steps:
(1) mixing a sample to be detected, water and acetonitrile, then sequentially mixing with anhydrous sodium acetate powder and anhydrous magnesium sulfate, centrifuging, taking supernatant, performing rotary evaporation, eluting and filtering to obtain a sample solution to be processed;
(2) preparing a series of standard solutions of fentanyl, remifentanil, sufentanil, alfentanil, acetylfentanil with gradually increased concentrations, sequentially carrying out HPLC-MS/MS detection on the standard solutions, and drawing a standard curve of the 7 components;
(3) and (3) carrying out HPLC-MS/MS detection on the to-be-detected sample solution, and substituting the response value of each component into the standard curve obtained in the step (2) to obtain the concentrations of the 7 components in the to-be-detected sample.
2. The method according to claim 1, wherein in the step (1), the sample to be detected, water, acetonitrile, anhydrous sodium acetate powder and anhydrous magnesium sulfate are used in a ratio of 1.80-2.20 g, 2-5 mL, 12-18 mL, 1.4-1.6 g, 5-8 g.
3. The method of claim 1, wherein the rotation speed of the centrifugation in the step (1) is 3500-4500 r/min, and the time of the centrifugation is 3-8 min.
4. The method according to claim 1, wherein the temperature of the rotary evaporation in the step (1) is 40-50 ℃, and the rotary evaporation is finished until no liquid exists in the sample.
5. The method according to claim 1, wherein the eluent eluted in step (1) comprises an aqueous formic acid solution containing ammonium acetate and acetonitrile; the ratio of the ammonium acetate-containing formic acid aqueous solution to acetonitrile is 8-12: 1, the concentration of ammonium acetate in the ammonium acetate-containing formic acid aqueous solution is 3-8 mmol/L, and the content of formic acid in the ammonium acetate-containing formic acid aqueous solution is 0.08% -0.12%.
6. The method according to claim 1, wherein the step (1) is carried out by filtration using a 0.22 μm nylon 66 organic filter.
7. The method according to any one of claims 1 to 6, wherein the sample to be detected in step (1) is a solid food or a liquid food.
8. The method of claim 1, wherein the chromatographic conditions for HPLC-MS/MS detection in step (3) are: adopting a Waters ACQUITY UPLClM BHE C18 chromatographic column, wherein the sample injection amount is 4-6 mu L, the chromatographic column temperature is 34-36 ℃, and the flow of a mobile phase is 0.2-0.4 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-1.0 min, 10% of mobile phase B; 1.1-3.0 min, 65% of mobile phase B; 3.1-4.0 min, 65% of mobile phase B; 4.1-6.0 min, 10% of mobile phase B.
9. The method of claim 1, wherein the chromatographic conditions for HPLC-MS/MS detection in step (3) are: adopting an ACQUITYUPLC @ HSST3 chromatographic column, wherein the sample volume is 4-6 mu L, the temperature of the chromatographic column is 34-36 ℃, and the flow rate of a mobile phase is 0.2-0.4 mL/min;
liquid chromatography uses mobile phase a: 0.1% formic acid-water solution containing 5mmol/L ammonium acetate and mobile phase B: acetonitrile is used as a mobile phase;
the gradient elution procedure was: 0-0.5 min, 10% of mobile phase B; 0.5-1.0 min, 35% of mobile phase B; 1.0-2.5 min, 35% of mobile phase B; 2.5-3.5 min, 35-10% of mobile phase B; 3.5-6.0 min, 10% of mobile phase B.
10. The method of claim 1, wherein the mass spectrometric conditions for HPLC-MS/MS detection in step (3) are:
a heatable electrospray ion source;
a positive ion scanning mode;
ion source voltage: 5000-6000V;
ion source temperature: 500-600 ℃;
air pressure of an air curtain: 24-26 psi;
collision air pressure: 8-12 psi;
spraying air pressure: 54-56 psi;
heating the air pressure: 54-56 psi;
an acquisition mode: multiple reaction monitoring mode MRM.
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