CN108760950A - A method of measuring metabolites of nitrofuran - Google Patents
A method of measuring metabolites of nitrofuran Download PDFInfo
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Abstract
The invention discloses a kind of methods measuring metabolites of nitrofuran, including derivative step：Sample to be tested is taken, the organic solution of dansyl chloride is added, heating water bath obtains derivative sample；Filtration step：Derivative sample is filtered, removal of impurities sample is obtained；Determination step：Removal of impurities sample is subjected to Liquid Chromatography-Tandem Mass Spectrometry measurement.The method of the measurement metabolites of nitrofuran, sample to be tested is derived using dansyl chloride, the nitrofuran dimethylamino naphthalene sulfonylamide compound generated after derivative does not allow facile hydrolysis, stability is good, therefore it need not use internal standard compound that can be measured, to reduce testing cost, while this method detection time shortens, more efficient.
Description
Technical field
The present invention relates to technical field of analytical chemistry more particularly to a kind of methods measuring metabolites of nitrofuran.
Background technology
Nitrofuran metabolites belong to one in detection of veterinary drugs in food project.The has a broad antifungal spectrum of Nitrofuran metabolites,
Sterilizing ability is strong, drug resistance is good, cheap, is once widely used in the infection of the cultivated animals such as poultry, domestic animal, pet and aquatic products
Disease prevention and treatment in, and as feed addictive for prevent and treat the pig caused by salmonella and Escherichia, ox,
The enterogastric diseases of poultry and honeybee are also used as domestic animal growth promoter.
Itrofurans active compound is metabolized rapidly in vivo, half-life short, therefore livestock and poultry etc. have used nitrofuran
It after object, is metabolized quickly in vivo, is not easy to be detected.Itrofurans active compound includes mainly furazolidone, furaltadone, furans
It is appropriate because of, four kinds of nitrofurazone, their major metabolite is 3- amino -2- oxazolidones, 3- amino -5- morpholino first respectively
Base -2- oxazolidones, 1-aminohydantoin, semicarbazides, these metabolites and protein combine it is more stable, can be in life
It is retained the long period in object tissue, therefore can reflect the residual shape of Nitrofuran metabolites using the detection of metabolites of nitrofuran
Condition.
Studies have shown that Nitrofuran metabolites have prodigious harmfulness to human body, being one kind has potential carcinogenic teratogenesis
With the substance of induced mutation.Therefore, countries in the world are very strict to the control of furans, and there are its Standard of Monitoring in various countries
Specific regulation.
The main method for detecting above-mentioned 4 kinds of metabolites of nitrofuran both at home and abroad now is liquid chromatography, liquid phase series connection matter
Spectrometry etc..Wherein, liquid phase tandem mass spectrometry is accuracy highest, most widely used detection method.
But the liquid phase tandem mass spectrometry for being currently used for detection base furans metabolin has the following defects：When measurement, use
2- nitrobenzaldehydes derive 4 kinds of metabolites of nitrofuran, generate group with imine moiety after derivative, are then measured.But it generates
Group with imine moiety is susceptible to hydrolysis, and stability is poor, needs to add internal standard compound, increases testing cost；Meanwhile after deriving
Sample retention time also do not grow, influence accuracy in detection.
Invention content
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of sides measuring metabolites of nitrofuran
Method derives sample to be tested using dansyl chloride, the nitrofuran dimethylamino naphthalene sulfonyl generated after derivative
Amine compounds do not allow facile hydrolysis, and stability is good, therefore need not use internal standard compound that can be measured, to reduce inspection
Cost is surveyed, while this method detection time shortens, it is more efficient.
The purpose of the present invention adopts the following technical scheme that realization：
A method of metabolites of nitrofuran is measured, including：
Derivative step：Sample to be tested is taken, the organic solution of dansyl chloride is added, heating water bath is derived
Sample；
Determination step：The derivative sample is subjected to Liquid Chromatography-Tandem Mass Spectrometry measurement.
Further, further include filtration step：The derivative sample is filtered, removal of impurities sample, the removal of impurities are obtained
Sample carries out Liquid Chromatography-Tandem Mass Spectrometry measurement again.
Further, in the filtration step, the derivative sample was carried out with the filter membrane that aperture is 0.2-0.8 μm
Filter.
Further, the aperture of the filter membrane is 0.45 μm.
Further, in the derivative step, the organic solution of the dansyl chloride is dimethylamino naphthalene
Sulfonic acid chloride acetonitrile solution.
Further, in the derivative step, 1-3mL water samples to be measured are taken, 0.1-0.3mL dimethylamino naphthalene sulfonyls are added
The organic solution of chlorine heats 50-70min in 80-100 DEG C of water-bath, obtains derivative sample.
Further, a concentration of 10000mg/L of the organic solution of the dansyl chloride.
Further, in the determination step, the determination condition of liquid chromatogram is：Waters ACQUITY UPLC
BEH C18Chromatographic column, 50mm x 2.1mm, 1.7 μm；40 DEG C of column temperature；1 μ L of sample size；Flow velocity is 0.3mL/min；Mobile phase A is
0.1% aqueous formic acid, Mobile phase B are methanol, gradient elution；
The condition of mass spectroscopy is：Cation scans；Capillary voltage 1.5kV；150 DEG C of ion source temperature；Remove solvent gas
500℃；Remove solvent stream amount 800L/h；Gas curtain throughput 50L/h；Multiple-reaction monitoring pattern detects.
Further, when liquid chromatogram measuring, the program of the gradient elution is：0-1min, 85%A；1-2min, 85%
A-15%A；2-3-min, 15%A；3-4min, 15%A-85%A；4-5min, 85%A.
Further, described to go solvent gas for nitrogen when mass spectroscopy；
The metabolites of nitrofuran includes：3- amino -2- oxazolidinyls ketone, 1-aminohydantoin, semicarbazides and 5-
Methyl morpholine -3- amino -2- oxazolidinyl ketone；Wherein, the ion pair parameter of 3- amino -2- oxazolidinyl ketone is 336/171,336/
236, quota ion parameter is 336/171；The ion pair parameter of 1-aminohydantoin is 349/171,349/236, it is quantitative from
Subparameter is 349/171；The ion pair parameter of semicarbazides is 309/309,309/171, and quota ion parameter is 309/171；5-
The ion pair parameter of methyl morpholine -3- amino -2- oxazolidinyl ketone is 435/170,435/234,435/171, quota ion parameter
It is 435/170.
Compared with prior art, the beneficial effects of the present invention are：
(1) method provided by the present invention for measuring metabolites of nitrofuran, at home and abroad reports and utilizes diformazan for the first time
Amino naphthalene sulfonyl chloride, which derives, measures 4 kinds of metabolites of nitrofuran, the nitrofuran dimethylamino naphthalene sulfonyl amination generated after derivative
It closes object and does not allow facile hydrolysis, stability is better than group with imine moiety, therefore need not use internal standard compound that can carry out subsequent measurements,
To reduce testing cost, while this method detection time shortens, more efficient.
(2) method provided by the present invention for measuring metabolites of nitrofuran, the derivative of metabolites of nitrofuran is in matter
It measures in concentration range 10-500 μ g/L and good linear relationship is presented with its peak area, correlation coefficient r is all higher than 0.9995；And
And according to 10 times of signal-to-noise ratio as its method detection limit, calculates its detection and be limited to 1 μ g/L, detection limit is low, high sensitivity；Meanwhile
The rate of recovery of the detection method is high, and precision is good.
Description of the drawings
The chromatogram for 4 kinds of metabolites of nitrofuran that Fig. 1 is provided by the embodiment of the present invention 1；
Fig. 2 is the derivatization process chemical formula of 4 kinds of metabolites of nitrofuran in the embodiment of the present invention 1.
Specific implementation mode
In the following, in conjunction with attached drawing and specific implementation mode, the present invention is described further, it should be noted that not
Under the premise of conflicting, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
A method of metabolites of nitrofuran is measured, including：
Derivative step：Sample to be tested is taken, the organic solution of dansyl chloride is added, heating water bath is derived
Sample；
Determination step：Derivative sample is subjected to Liquid Chromatography-Tandem Mass Spectrometry measurement.
Further include filtration step as further embodiment：Derivative sample is filtered, removal of impurities sample is obtained,
Removal of impurities sample carries out Liquid Chromatography-Tandem Mass Spectrometry measurement again.
As further embodiment, in filtration step, derivative sample is carried out with the filter membrane that aperture is 0.2-0.8 μm
Filtering.
As further embodiment, the aperture of filter membrane is 0.45 μm.
As further embodiment, in derivative step, the organic solution of dansyl chloride is diformazan ammonia
Base naphthalene sulfonyl chloride acetonitrile solution.
1-3mL water samples to be measured are taken in derivative step as further embodiment, 0.1-0.3mL diformazan ammonia is added
The organic solution of base naphthalene sulfonyl chloride heats 50-70min in 80-100 DEG C of water-bath, obtains derivative sample.
As further embodiment, a concentration of 10000mg/L of the organic solution of dansyl chloride.
As further embodiment, in determination step, the determination condition of liquid chromatogram is：Waters ACQUITY
UPLC BEH C18Chromatographic column, 50mm x 2.1mm, 1.7 μm；40 DEG C of column temperature；1 μ L of sample size；Flow velocity is 0.3mL/min；Flowing
Phase A is 0.1% aqueous formic acid, and Mobile phase B is methanol, gradient elution；
The condition of mass spectroscopy is：Cation scans；Capillary voltage 1.5kV；150 DEG C of ion source temperature；Remove solvent gas
500℃；Remove solvent stream amount 800L/h；Gas curtain throughput 50L/h；Multiple-reaction monitoring pattern detects.
As further embodiment, when liquid chromatogram measuring, the program of gradient elution is：0-1min, 85%A；1-
2min, 85%A-15%A；2-3-min, 15%A；3-4min, 15%A-85%A；4-5min, 85%A.(that is, 0-
When 1min, mobile phase is made of 85%A and 15%B；When 1-2min, mobile phase is by 85%A-15%A and 15%B-85%B groups
At；Remaining period is similarly.)
When carrying out mass spectroscopy, detection method is scanned using cation, is made using 0.1% aqueous formic acid and methanol
For mobile phase, be conducive to the formation of cation, and used when gradient elution and be incremented to high organic Phase Proportion from low organic Phase Proportion,
Be conducive to the elution of substance to be detected and obtain good retention time.
As further embodiment, when mass spectroscopy, it is nitrogen to remove solvent gas；
Metabolites of nitrofuran includes：3- amino -2- oxazolidinyls ketone, 1-aminohydantoin, semicarbazides and 5- methyl
Morpholine -3- amino -2- oxazolidinyl ketone；Wherein, the ion pair parameter of 3- amino -2- oxazolidinyl ketone is 336/171,336/236,
Quota ion parameter is 336/171；The ion pair parameter of 1-aminohydantoin is 349/171,349/236, quota ion ginseng
Number is 349/171；The ion pair parameter of semicarbazides is 309/309,309/171, and quota ion parameter is 309/171；5- methyl
The ion pair parameter of morpholine -3- amino -2- oxazolidinyl ketone is 435/170,435/234,435/171, and quota ion parameter is
435/170。
The method for the measurement metabolites of nitrofuran that the embodiment of the present invention is provided, is treated using dansyl chloride
Sample is derived, and the nitrofuran dimethylamino naphthalene sulfonylamide compound generated after derivative does not allow facile hydrolysis, stability ratio
Group with imine moiety is good, therefore need not use internal standard compound that can carry out subsequent measurements, to reduce testing cost, simultaneously
This method detection time shortens, more efficient.Also, the derivative of 4 kinds of metabolites of nitrofuran is in mass concentration range 10-
Good linear relationship is presented with its peak area in 500 μ g/L, correlation coefficient r is all higher than 0.9995；Also, believe according to 10 times
It makes an uproar and is limited to 1 μ g/L than as its method detection limit, calculating its detection, detection limit is low, high sensitivity；Meanwhile the detection method
The rate of recovery is high, and precision is good.
It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments
It can be obtained by buying pattern outside fixed.
Embodiment 1：
A method of metabolites of nitrofuran is measured, including：
Derivative step：1mL water samples to be measured are taken, the dansyl chloride acetonitrile solution of 0.1mL 10000mg/L is added,
60min is heated in 100 DEG C of water-bath, obtains derivative sample (as shown in Fig. 2, deriving for 4 kinds of metabolites of nitrofuran
Journey)；
Filtration step：Derivative sample is filtered with the filter membrane that aperture is 0.45 μm, obtains removal of impurities sample；
Determination step：Removal of impurities sample is subjected to Liquid Chromatography-Tandem Mass Spectrometry measurement；
Liquid phase chromatogram condition:Waters ACQUITY UPLC BEH C18Chromatographic column, 50mm x 2.1mm, 1.7 μm；Column temperature
40℃；1 μ L of sample size；Flow velocity is 0.3mL/min；Mobile phase A is 0.1% aqueous formic acid, and Mobile phase B is methanol, and gradient is washed
It is de-：0-1min, 85%A；1-2min, 85%A-15%A；2-3-min, 15%A；3-4min, 15%A-85%A；4-5min,
85%A；
Mass Spectrometry Conditions:Cation scans；Capillary voltage 1.5kV；150 DEG C of ion source temperature；Remove 500 DEG C of solvent gas；It goes
Solvent gas (nitrogen) flow 800L/h；Gas curtain throughput 50L/h；Multiple-reaction monitoring (MRM) mode detection；3- amino -2- oxazoles
The ion pair parameter of alkyl ketone is 336/171,336/236, and quota ion parameter is 336/171；1-aminohydantoin from
Son is 349/171,349/236 to parameter, and quota ion parameter is 349/171；The ion pair parameter of semicarbazides be 309/309,
309/171, quota ion parameter is 309/171；The ion pair parameter of 5- methyl morpholine -3- amino -2- oxazolidinyl ketone is 435/
170,435/234,435/171, quota ion parameter is 435/170.
For measurement result as shown in Figure 1, can be obtained from Fig. 1, the appearance effect of 4 kinds of metabolites of nitrofuran is good.
Embodiment 2：
Embodiment 2 difference from example 1 is that：
In derivative step, 2mL water samples to be measured are taken, the dansyl chloride acetonitrile of 0.2mL 10000mg/L is added
Solution heats 50min in 90 DEG C of water-bath.
It is other identical as specific embodiment 1.
Embodiment 3：
Embodiment 3 difference from example 1 is that：In derivative step, 3mL water samples to be measured are taken, 0.3mL is added
The dansyl chloride acetonitrile solution of 10000mg/L, 70min is heated in 80 DEG C of water-bath.
It is other identical as specific embodiment 1.
Effect assessment and performance detection
1, the range of linearity and detection limit
It is configured to 5 μ g/L, 10 μ g/L, 20 μ g/L, 50 μ g/L, 100 μ with the metabolites of nitrofuran standard solution of 10mg/L
Metabolites of nitrofuran each 1.0mL of standard curve liquid of g/L, adds 0.1mL10000mg/L dansyl chloride acetonitriles molten
Liquid, the water-bath 60min in 100 DEG C of water-baths；After derivative Liquid Chromatography-Tandem Mass Spectrometry measurement is carried out according to the method for embodiment 1.
The result shows that establishing curve, the derivative of metabolites of nitrofuran with the quota ion of 4 kinds of metabolites of nitrofuran
Good linear relationship (referring to the following table 1) is presented with its peak area in 10 μ g/L-500 μ g/L of mass concentration range, it is related
Coefficient r is all higher than 0.9995.Detection limit is generally using method detection limit as its detection limit, according to 10 times of signal-to-noise ratio as its method
Detection limit calculates its detection and is limited to 1 μ g/L.
The linear equation of 14 kinds of metabolites of nitrofuran of table
| Linear equation | Related coefficient | |
| 3- amino -2- oxazolidinyl ketone | Y=8026.27x+9852.27 | 0.9999 |
| 1-aminohydantoin | Y=4935.22x+5986.29 | 0.9998 |
| Semicarbazides | Y=1765.17x+76.23 | 0.9999 |
| 5- methyl morpholine -3- amino -2- oxazolidinyl ketone | Y=3954.32x+1388.55 | 0.9996 |
2, the rate of recovery and precision
It selects by measuring the water sample without containing metabolites of nitrofuran, is divided into three groups.
Three groups of samples add basic, normal, high three concentration of 10 μ g/L, 20 μ g/L, 50 μ g/L respectively, respectively according to embodiment 1-
3 method is added rate of recovery experiment, calculates its rate of recovery.
Parallel determination three above concentration 3 times calculates its relative standard deviation RSD, the gained rate of recovery and precision result
It is shown in Table 2.
2 rate of recovery of table and Precision Experiment result
It can be obtained from the data in table 1, the assay method rate of recovery for the metabolites of nitrofuran that the embodiment of the present invention is provided
Height, precision is good, and wherein embodiment 1 obtains best test result, is most preferred embodiment.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. a kind of method measuring metabolites of nitrofuran, which is characterized in that including：
Derivative step：Sample to be tested is taken, the organic solution of dansyl chloride is added, heating water bath obtains derivative sample；
Determination step：The derivative sample is subjected to Liquid Chromatography-Tandem Mass Spectrometry measurement.
2. the method for measuring metabolites of nitrofuran as described in claim 1, which is characterized in that further include filtration step：It will
The derivative sample is filtered, and obtains removal of impurities sample, and the removal of impurities sample carries out Liquid Chromatography-Tandem Mass Spectrometry measurement again.
3. the method for measuring metabolites of nitrofuran as claimed in claim 2, which is characterized in that in the filtration step,
The derivative sample is filtered with the filter membrane that aperture is 0.2-0.8 μm.
4. the method for measuring metabolites of nitrofuran as claimed in claim 3, which is characterized in that the aperture of the filter membrane is
0.45μm。
5. the method for measuring metabolites of nitrofuran as described in claim 1, which is characterized in that in the derivative step,
The organic solution of the dansyl chloride is dansyl chloride acetonitrile solution.
6. the method for measuring metabolites of nitrofuran as described in claim 1, which is characterized in that in the derivative step,
1-3mL water samples to be measured are taken, the organic solution of 0.1-0.3mL dansyl chlorides is added, are added in 80-100 DEG C of water-bath
Hot 50-70min obtains derivative sample.
7. the method for measuring metabolites of nitrofuran as claimed in claim 6, which is characterized in that the dimethylamino naphthalene sulfonyl
A concentration of 10000mg/L of the organic solution of chlorine.
8. the method for measuring metabolites of nitrofuran as described in claim 1, which is characterized in that in the determination step,
The determination condition of liquid chromatogram is：Waters ACQUITY UPLC BEH C18Chromatographic column, 50mm x 2.1mm, 1.7 μm；Column temperature
40℃；1 μ L of sample size；Flow velocity is 0.3mL/min；Mobile phase A is 0.1% aqueous formic acid, and Mobile phase B is methanol, and gradient is washed
It is de-；
The condition of mass spectroscopy is：Cation scans；Capillary voltage 1.5kV；150 DEG C of ion source temperature；Remove solvent gas 500
℃；Remove solvent stream amount 800L/h；Gas curtain throughput 50L/h；Multiple-reaction monitoring pattern detects.
9. the method for measuring metabolites of nitrofuran as claimed in claim 8, which is characterized in that when liquid chromatogram measuring, institute
The program for stating gradient elution is：0-1min, 85%A；1-2min, 85%A-15%A；2-3-min, 15%A；3-4min, 15%
A-85%A；4-5min, 85%A.
10. the method for measuring metabolites of nitrofuran as claimed in claim 8, which is characterized in that described to go when mass spectroscopy
Solvent gas is nitrogen；
The metabolites of nitrofuran includes：3- amino -2- oxazolidinyls ketone, 1-aminohydantoin, semicarbazides and 5- methyl
Morpholine -3- amino -2- oxazolidinyl ketone；Wherein, the ion pair parameter of 3- amino -2- oxazolidinyl ketone is 336/171,336/236,
Quota ion parameter is 336/171；The ion pair parameter of 1-aminohydantoin is 349/171,349/236, quota ion ginseng
Number is 349/171；The ion pair parameter of semicarbazides is 309/309,309/171, and quota ion parameter is 309/171；5- methyl
The ion pair parameter of morpholine -3- amino -2- oxazolidinyl ketone is 435/170,435/234,435/171, and quota ion parameter is
435/170。
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