CN109613135A - The rapid detection method of N- methyl carbamyl adduct in a kind of blood - Google Patents
The rapid detection method of N- methyl carbamyl adduct in a kind of blood Download PDFInfo
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- CN109613135A CN109613135A CN201811581413.8A CN201811581413A CN109613135A CN 109613135 A CN109613135 A CN 109613135A CN 201811581413 A CN201811581413 A CN 201811581413A CN 109613135 A CN109613135 A CN 109613135A
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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
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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
- G01N30/06—Preparation
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses a kind of rapid detection methods of N- methyl carbamyl adduct in blood, method includes the following steps: the Solid Phase Extraction of sample is handled；The foundation of liquid chromatography-tandem mass spectrometry；The foundation of standard curve；Sample measurement.Sample is handled through Solid Phase Extraction, high performance liquid chromatography-tandem mass technology is analyzed, and uses internal standard method, is measured under the conditions of electric spray ion source ionization and multiple-reaction monitoring pattern.Rapid detection method of the invention has the advantages that quick, accurate, sensitive, of low pollution, low cost, the accurate quick detection suitable for a large amount of samples.
Description
Technical field
The present invention relates to medicine technology fields, it particularly relates in a kind of blood N- methyl carbamyl adduct it is quick
Detection method.
Background technique
N- methyl carbamyl adduct (N-methylcarbamoyl adduct) is dimethylformamide (DMF) in blood
Metabolin.DMF is widely used in fields such as China's medication chemistries, and Work places DMF mainly enters body through respiratory tract and skin,
Lungs, liver and kidney and other organs are damaged, serious person can lead to death.DMF has become in Chinese industrial poisoning often
One of poisonous substance seen.The carcinogenic substance inventory edit reference that international cancer research institution, the World Health Organization in 2017 announces,
Dimethylformamide is in 2A class carcinogenic substance inventory.Carry out DMF biological marker analyte detection, for preventing and controlling Work places
DMF poisoning, protects the health of labourer to be of great significance.Since blood of human body red blood cell renewal time is up to 4 months, N- first
Base carbamyl adduct once being formed, can maintain metastable level in a longer period of time, studies have shown that generation in DMF body
It thanks to the N- methyl carbamyl adduct that product methyl isocyanate and interaction of Hb are formed, can be used as reflection DMF occupation
The biomarker of exposure level.The detection of N- methyl carbamyl adduct in blood, can be by edman degradation, by adduction
Object is degraded in 3- methyl-isopropyl second sour urea (3-methyl-5-isopropylhydantoin), with gas-chromatography-matter
Spectrometry, gas chromatography are measured.
Existing gas chromatography-mass spectrography, gas chromatography treatment process are cumbersome, and qualitative poor reliability, sensitivity is low, time-consuming
Long, pollution weight is at high cost.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of the fast of N- methyl carbamyl adduct in blood
Fast detection method.
To realize the above-mentioned technical purpose, the technical scheme of the present invention is realized as follows:
The rapid detection method of N- methyl carbamyl adduct in a kind of blood, comprising the following steps:
S1. the processing of sample
S11. blood sample 1-10 mL is collected with the heparin tube of anticoagulant heparin, centrifugation discards blood plasma, and splitting erythrocyte adds acetone
Solution (concentrated hydrochloric acid containing 2%), sedimentation centrifugation abandon supernatant, wash and dry, obtain hemoglobin；
S12. the hemoglobin for accurately weighing 0.01-0.2g is placed in centrifuge tube, and it is molten that 3- methyl-isobutyl glycolylurea internal standard is added
Liquid is degraded after adding hydrochloric acid-acetic acid (2:1, V/V) solution, the solution progress purified treatment after degradation is obtained to be measured
Sample liquid, then the sample solution to be tested is transferred to be measured in sample bottle；
S13. 3- methyl-isobutyl glycolylurea inner mark solution is added to another centrifuge tube, it is molten adds hydrochloric acid-acetic acid (2:1, V/V)
It degrades after liquid, the solution after degradation is subjected to purified treatment and obtains blank sample liquid, then blank sample liquid is transferred to sample bottle
In it is to be measured；
The foundation of S2 liquid chromatography-tandem mass spectrometry
Chromatographic condition: chromatographic column: C18 chromatographic column；
Mass Spectrometry Conditions: ionization mode: electric spray ion source (ESI+)；
Multiple-reaction monitoring pattern: sour urea monitoring 72.0/157.1 (quantitative), 129.1/157.1 in 3- methyl-isopropyl second；3- first
Base-isobutyl group glycolylurea monitors 86.0/171.1；
S3. the foundation of standard curve
Urea standard series working solution sour in 3- methyl-isopropyl second and internal standard compound 3- methyl-isobutyl glycolylurea are measured, with
The peak area ratio of sour urea and internal standard 3- methyl-isobutyl glycolylurea is ordinate in 3- methyl-isopropyl second, different with 3- methyl-
Sour urea standard series working solution concentration is that abscissa draws standard curve in propyl second；
S4. sample measures
By the sample solution to be tested and the blank sample liquid sequentially determining sample introduction, the peak area ratio of determinand and internal standard compound is obtained,
The concentration of sour urea in 3- methyl-isopropyl second in measurement liquid is obtained according to standard curve, and obtains N- methyl carbamyl in sample
The concentration of adduct.
Further, splitting erythrocyte described in the step S11 is first clean red blood cell with physiological saline, then with distilling
Water cracks under ultrasonic state.
Further, drying means described in the step S11 is to be dried with nitrogen or depressurize 30-65 DEG C of drying in baking oven.
Further, the concentration of 3- methyl-isobutyl glycolylurea inner mark solution described in the step S12 and step S13 is
The volume of 40nmol/mL, the 3- methyl-isobutyl glycolylurea inner mark solution are 250 μ L, and the hydrochloric acid-acetic acid (2:1, V/V) is molten
The volume of liquid is 4.75mL.
Further, centrifuge tube is placed in 70-100 DEG C of water-bath in degradation described in the step S12 and step S13 and is added
Thermal degradation 1h, the purified treatment are to take 200 μ L to 96 orifice plates, and 600 μ L1% formic acid acetonitrile solutions are added, mix, control vacuum
Pump pressure flows out sample in 2 ~ 4min, is acid in 3- methyl-isopropyl second by N- methyl carbamyl adduct fully degraded
Urea.
Further, chromatographic condition described in the step S2 is column temperature: 25-45 DEG C；Mobile phase A: 0.1% formic acid；Flowing
Phase B: acetonitrile；Gradient elution program are as follows: 0min ~ 3min, A by 90% ~ 10%, 3min ~ 3.2min, A by 10% ~ 10%, 3.2min ~
3.5min, A are by 10% ~ 90%, 3.5min ~ 4.0min, and A is by 90% ~ 90%；Flow velocity: 0.25mL/min；Sample volume: 5 μ L.
Further, Mass Spectrometry Conditions described in the step S2 are capillary voltage: 3.5kv；Source temperature: 150 DEG C；Desolventizing
Temperature: 350 DEG C；Desolvention gas velocity: 800L/h.
Further, the concentration of sour urea standard series working solution is in 3- methyl-isopropyl second described in the step S3
0.01nmol/mL, 0.05nmol/mL, 0.1nmol/mL, 0.5nmol/mL, 1.0nmol/mL, 2.0nmol/mL, the internal standard
Object 3- methyl-isobutyl glycolylurea concentration is 0.5nmol/mL.
The rapid detection method of N- methyl carbamyl adduct in a kind of blood of the present invention using Solid Phase Extraction, surpasses
High performance liquid chromatography-tandem mass technology analysis, using internal standard method, in electric spray ion source ionization and multiple-reaction monitoring pattern item
It is quantitative determined under part.
Beneficial effects of the present invention: using Solid Phase Extraction that urea sour in 3- methyl-isopropyl second and matrix interference object is effective
Separation, while internal standard 3- methyl-isobutyl glycolylurea can also be efficiently separated with matrix interference object, reduced pollution, improved sensitivity,
It is quantitative more accurate, it is purified using 96 orifice plates, is quickly detected.
Specific embodiment
S3. the foundation of standard curve
Embodiment 1:
S1. the processing of sample
S11. certain 18, Leather Factory's dimethylformamide occupational exposure post worker's blood is acquired with the heparin tube of anticoagulant heparin
5ml is centrifuged 15min, discards blood plasma；Twice with physiology salt washing red blood cell, it is then cracked under ultrasonic state with 1mL distilled water
Red blood cell；It is slowly added to 15mL pre-cooling acetone soln (concentrated hydrochloric acid containing 2%)；The albumen of sedimentation is centrifuged 5min, discards supernatant liquid
Body, then the acetone soln described in 15mL clean 3 times, then are cleaned with ethyl acetate 15mL, and nitrogen is dry；
S12. the hemoglobin for accurately weighing 0.1g is placed in 15mL centrifuge tube, and the 3- methyl-isobutyl of 40nmol/mL is added
250 μ L of glycolylurea inner mark solution, adds hydrochloric acid-acetic acid (2:1, V/V) solution 4.75mL, and oscillation mixes 3min；Centrifuge tube is set
Heating degradation 1h, takes out cooling in 100 DEG C of water-baths；Solution after degradation is mixed, 200 μ L to 96 orifice plates are taken, 600 μ are added
L1% formic acid acetonitrile solution controls vacuum pump pressure, flows out sample in 2 ~ 4min, obtains the sample solution to be tested after mixing, will be to test sample
Liquid is transferred to be measured in sample bottle；
S13. the 250 μ L of 3- methyl-isobutyl glycolylurea inner mark solution of 40nmol/mL is added to another 15mL centrifuge tube, adds
Hydrochloric acid-acetic acid (2:1, V/V) solution 4.75mL, oscillation mix 3min；Centrifuge tube is placed in heating degradation 1h in 100 DEG C of water-baths,
Take out cooling；Solution after degradation is mixed, 200 μ L to 96 orifice plates are taken, 600 μ L1% formic acid acetonitrile solutions are added, are after mixing
Blank sample liquid is obtained, blank sample liquid is transferred to be measured in sample bottle；
The foundation of S2 liquid chromatography-tandem mass spectrometry
Chromatographic condition are as follows: chromatographic column: C18 chromatographic column (5 μm, 100,2.1mm i.d. × 150mm)；Column temperature: 35 DEG C；Mobile phase
A:0.1% formic acid；Mobile phase B: acetonitrile；Gradient elution program are as follows: 0 min ~ 3min, A by 90% ~ 10%, 3min ~ 3.2min, A by
10% ~ 10%, 3.2min ~ 3.5min, A are by 10% ~ 90%, 3.5min ~ 4.0min, and A is by 90% ~ 90%；Flow velocity: 0.25mL/min；Into
Sample amount: 5 μ L；
Mass Spectrometry Conditions are as follows: ionization mode: electric spray ion source (ESI+)；Capillary voltage: 3.5kv；Source temperature: 150 DEG C；Desolventizing
Temperature: 350 DEG C；Desolvention gas velocity: 800L/h；
Multiple-reaction monitoring pattern: sour urea monitoring 72.0/157.1 (quantitative), 129.1/157.1 in 3- methyl-isopropyl second；3- first
Base-isobutyl group glycolylurea monitors 86.0/171.1；
S3. the foundation of standard curve
Prepare sour urea concentration in standard curve each point 3- methyl-isopropyl second be 0.01nmol/mL, 0.05nmol/mL,
0.1nmol/mL, 0.5nmol/mL, 1.0nmol/mL, 2.0nmol/mL, internal standard compound 3- methyl-isobutyl glycolylurea concentration are
0.5nmol/mL is respectively successively carried out urea standard series working solution sour in 3- methyl-isopropyl second by low concentration to high concentration
Measurement；Using the peak area ratio of urea sour in 3- methyl-isopropyl second and internal standard 3- methyl-isobutyl glycolylurea as ordinate, with 3-
Sour urea standard series working solution concentration is that abscissa draws standard curve in methyl-isopropyl second；
S4. sample measures
Sample the sample solution to be tested and blank the sample solution to be tested are successively measured, the peak area ratio of determinand and internal standard compound is obtained,
The concentration of sour urea in 3- methyl-isopropyl second in measurement liquid is obtained according to standard curve, and obtains N- methyl carbamyl in sample
The concentration table 1 of adduct.
The testing result of the concentration of 1 N- methyl carbamyl adduct of table
Embodiment 2:
S1. the processing of sample
S11. experiment mouse blood 3ml is collected with the heparin tube of anticoagulant heparin, is centrifuged 15min, discards blood plasma；Use physiological saline
It washes red blood cell twice, then uses 1mL distilled water splitting erythrocyte under ultrasonic state；It is slowly added to 15mL pre-cooling acetone soln
(concentrated hydrochloric acid containing 2%)；The albumen of sedimentation is centrifuged 5min, discards supernatant liquid, then the acetone soln described in 15mL cleans 3 times,
It is cleaned again with ethyl acetate 15mL, is placed in 45 DEG C of decompression baking ovens and dries to dry；
S12. the hemoglobin for accurately weighing 0.05g is placed in 15mL centrifuge tube, and the 3- methyl-isobutyl of 40nmol/mL is added
250 μ L of glycolylurea inner mark solution, adds hydrochloric acid-acetic acid (2:1, V/V) solution 4.75mL, and oscillation mixes 3min；Centrifuge tube is set
Heating degradation 1h, takes out cooling in 100 DEG C of water-baths；Solution after degradation is mixed, 200 μ L to 96 orifice plates are taken, 600 μ are added
L1% formic acid acetonitrile solution, is uniformly mixed so as to obtain the sample solution to be tested, the sample solution to be tested is transferred to be measured in sample bottle；
S13. the 250 μ L of 3- methyl-isobutyl glycolylurea inner mark solution of 40nmol/mL is added to another 15mL centrifuge tube, adds
Hydrochloric acid-acetic acid (2:1, V/V) solution 4.75mL, oscillation mix 3min；Centrifuge tube is placed in heating degradation 1h in 100 DEG C of water-baths,
Take out cooling；Solution after degradation is mixed, 200 μ L to 96 orifice plates are taken, 600 μ L1% formic acid acetonitrile solutions are added, after mixing
To blank sample liquid, blank sample liquid is transferred to be measured in sample bottle；
The foundation of S2 liquid chromatography-tandem mass spectrometry
Chromatographic condition are as follows: chromatographic column: C18 chromatographic column (5 μm, 100,2.1mm i.d. × 150mm)；Column temperature: 35 DEG C；Mobile phase
A:0.1% formic acid；Mobile phase B: acetonitrile；Gradient elution program are as follows: 0 min ~ 3min, A by 90% ~ 10%, 3min ~ 3.2min, A by
10% ~ 10%, 3.2min ~ 3.5min, A are by 10% ~ 90%, 3.5min ~ 4.0min, and A is by 90% ~ 90%；Flow velocity: 0.25mL/min；Into
Sample amount: 5 μ L；
Mass Spectrometry Conditions are as follows: ionization mode: electric spray ion source (ESI+)；Capillary voltage: 3.5kv；Source temperature: 150 DEG C；Desolventizing
Temperature: 350 DEG C；Desolvention gas velocity: 800L/h；
Multiple-reaction monitoring pattern: sour urea monitoring 72.0/157.1 (quantitative), 129.1/157.1 in 3- methyl-isopropyl second；3- first
Base-isobutyl group glycolylurea monitors 86.0/171.1；
S3. the foundation of standard curve
Prepare sour urea concentration in standard curve each point 3- methyl-isopropyl second be 0.01nmol/mL, 0.05nmol/mL,
0.1nmol/mL, 0.5nmol/mL, 1.0nmol/mL, 2.0nmol/mL, internal standard compound 3- methyl-isobutyl glycolylurea concentration are
0.5nmol/mL, respectively by urea standard series working solution sour in 3- methyl-isopropyl second from low concentration to high concentration successively to step
Rapid S2 the method is measured；With the peak area ratio of urea and internal standard 3- methyl-isobutyl glycolylurea sour in 3- methyl-isopropyl second
Value is ordinate, draws standard curve using urea standard series working solution concentration sour in 3- methyl-isopropyl second as abscissa；
S4. sample measures
The sample the sample solution to be tested and the blank the sample solution to be tested are successively measured sample introduction to step S2 the method, obtained
The peak area ratio of determinand and internal standard compound obtains in measurement liquid the dense of sour urea in 3- methyl-isopropyl second according to standard curve
Degree, and obtain the concentration table 2 of N- methyl carbamyl adduct in sample.
The testing result of the concentration of 2 N- methyl carbamyl adduct of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. the rapid detection method of N- methyl carbamyl adduct in a kind of blood, which comprises the following steps:
S1. the processing of sample
S11. blood sample 1-10 mL is collected with the heparin tube of anticoagulant heparin, centrifugation discards blood plasma, and splitting erythrocyte adds acetone
Solution (concentrated hydrochloric acid containing 2%), sedimentation centrifugation abandon supernatant, wash and dry, obtain hemoglobin；
S12. the hemoglobin for accurately weighing 0.01-0.2g is placed in centrifuge tube, and it is molten that 3- methyl-isobutyl glycolylurea internal standard is added
Liquid is degraded after adding hydrochloric acid-acetic acid (2:1, V/V) solution, the solution progress purified treatment after degradation is obtained to be measured
Sample liquid, then the sample solution to be tested is transferred to be measured in sample bottle；
S13. 3- methyl-isobutyl glycolylurea inner mark solution is added to another centrifuge tube, it is molten adds hydrochloric acid-acetic acid (2:1, V/V)
It degrades after liquid, the solution after degradation is subjected to purified treatment and obtains blank sample liquid, then blank sample liquid is transferred to sample bottle
In it is to be measured；
The foundation of S2 liquid chromatography-tandem mass spectrometry
Chromatographic condition: chromatographic column: C18 chromatographic column；
Mass Spectrometry Conditions: ionization mode: electric spray ion source (ESI+)；
Multiple-reaction monitoring pattern: sour urea monitoring 72.0/157.1 (quantitative), 129.1/157.1 in 3- methyl-isopropyl second；3- first
Base-isobutyl group glycolylurea monitors 86.0/171.1；
S3. the foundation of standard curve
Urea standard series working solution sour in 3- methyl-isopropyl second and internal standard compound 3- methyl-isobutyl glycolylurea are measured, with
The peak area ratio of sour urea and internal standard 3- methyl-isobutyl glycolylurea is ordinate in 3- methyl-isopropyl second, different with 3- methyl-
Sour urea standard series working solution concentration is that abscissa draws standard curve in propyl second；
S4. sample measures
By the sample solution to be tested and the blank sample liquid sequentially determining sample introduction, the peak area ratio of determinand and internal standard compound is obtained,
The concentration of sour urea in 3- methyl-isopropyl second in measurement liquid is obtained according to standard curve, and obtains N- methyl carbamyl in sample
The concentration of adduct.
2. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
Splitting erythrocyte described in the step S11 is first to clean red blood cell with physiological saline, then split under ultrasonic state with distilled water
Solution.
3. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
Drying means described in the step S11 is to be dried with nitrogen or depressurize 30-65 DEG C of drying in baking oven.
4. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
The concentration of 3- methyl-isobutyl glycolylurea inner mark solution described in the step S12 and step S13 is 40nmol/mL, the 3- first
Base-isobutyl group glycolylurea inner mark solution volume is 250 μ L, and the volume of hydrochloric acid-acetic acid (2:1, the V/V) solution is 4.75mL.
5. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
Centrifuge tube is placed in heating degradation 1h, the purification in 70-100 DEG C of water-bath in degradation described in the step S12 and step S13
Processing is added 600 μ L1% formic acid acetonitrile solutions, mixes, control vacuum pump pressure to take 200 μ L to 96 orifice plates, make sample 2 ~
4min outflow.
6. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
Chromatographic condition described in the step S2 is column temperature: 25-45 DEG C；Mobile phase A: 0.1% formic acid；Mobile phase B: acetonitrile；Gradient elution
Program are as follows: 0min ~ 3min, A by 90% ~ 10%, 3min ~ 3.2min, A by 10% ~ 10%, 3.2min ~ 3.5min, A by 10% ~ 90%,
3.5min ~ 4.0min, A are by 90% ~ 90%；Flow velocity: 0.25mL/min；Sample volume: 5 μ L.
7. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
Mass Spectrometry Conditions described in the step S2 are capillary voltage: 3.5kv；Source temperature: 150 DEG C；Desolventizing temperature: 350 DEG C；Desolventizing
Gas velocity: 800L/h.
8. the rapid detection method of N- methyl carbamyl adduct in a kind of blood according to claim 1, which is characterized in that
In 3- methyl-isopropyl second described in the step S3 concentration of sour urea standard series working solution be 0.01nmol/mL,
0.05nmol/mL, 0.1nmol/mL, 0.5nmol/mL, 1.0nmol/mL, 2.0nmol/mL, the internal standard compound 3- methyl-isobutyl
Base glycolylurea concentration is 0.5nmol/mL.
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| CN115078563A (en) * | 2022-05-06 | 2022-09-20 | 天津国科医工科技发展有限公司 | Method for detecting methyl isocyanate |
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Application publication date: 20190412 |