CN108535378A - Gas Chromatography-Negative chemical source-tandem mass spectrum detection method of ethiprole and its metabolite amide ethiprole in birds, beasts and eggs - Google Patents
Gas Chromatography-Negative chemical source-tandem mass spectrum detection method of ethiprole and its metabolite amide ethiprole in birds, beasts and eggs Download PDFInfo
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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
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Abstract
Chemical source tandem mass spectrum detection method is born the invention discloses the gas-chromatography of ethiprole in a kind of birds, beasts and eggs and its metabolite amide ethiprole, and the present invention being capable of the residual quantity of ethiprole and its metabolite amide ethiprole in Accurate Determining birds, beasts and eggs.Birds, beasts and eggs sample adds acetonitrile extraction object to obtain liquid to be clean, liquid to be clean distributes grease removal and matrix dispersion purification pipe purification through n-hexane liquid liquid, object compares carry out qualitative analysis in the case where gas-chromatography bears chemical source tandem mass spectrometer multiple-reaction monitoring pattern with retention time and ion pair information, inner mark method ration, this method analyze speed is fast, high sensitivity, reproducibility and accuracy are good, to ensure that quality of egg provides safely new detection method.
Description
Technical field
The invention belongs to field of food detection, are related to QuEChERS extraction and cleanings-Gas Chromatography-Negative chemical source-series connection matter
The detection method of ethiprole and its metabolite amide ethiprole in spectrometry (GC-NCI-MS/MS), in particular to a kind of birds, beasts and eggs,
It is particularly suitable for the birds, beasts and eggs such as egg.
Background technology
Ethiprole is phenyl pyrazoles novel high-activity insecticide, has broad spectrum disinfestation effect, later stage the 1990s
It is promoted the use of on a large scale in China.Animal experiment study shows that taken long-term ethiprole may damage liver, thyroid gland and kidney
It is dirty.Ethiprole can generate fluorine formonitrile HCN, the vulcanization fluorine worm of toxicity bigger by photodissociation, reduction, oxidation, hydrolysis in the environment
Nitrile, ethiprole sulfone and amide ethiprole.
Codex Alimentary Commission（CAC）It is 0.02 to define the residue limits of ethiprole and its metabolite in eggs
Mg/kg, ethiprole residue limits are 0.02 mg/kg in regulation egg in Japanese positive list.In China GB2763-2016 only
Provide plant-derived Fluorine in Foods worm nitrile its metabolite fluorine formonitrile HCN, vulcanization ethiprole, ethiprole sulfone residue limits be 0.02-
0.1 mg/kg does not include its hydrolysate amide ethiprole.The Ministry of Agriculture of China, Ministry of Industry and Information and Chinese Ministry of Environmental Protection were in joint hair in 2009
Cloth No. 1157 bulletins are, it is specified that ethiprole is only allowed in the dry land seed pelleting of the parts such as peanut and corn and to use.
Currently, existing standard such as GB/T20769-2008, SN/T1982-2007, SN/T4039-2014 etc. are only for fluorine
The assay method that worm nitrile defines does not make regulation to its metabolite.The metabolite of existing document concern is mainly fluorine
Formonitrile HCN, vulcanization ethiprole, ethiprole sulfone, it is few to the detection of hydrolysis metabolites amide ethiprole.Therefore, it is necessary to establish fluorine worm
The detection method of nitrile and its hydrolysis metabolites amide ethiprole is to make up blank.
The existing document report of ethiprole residues detecton mainly has gas chromatography（GC）, the mono- quadrupole rod matter of gas-chromatography-
Spectrometry（GC-MS）, Liquid Chromatography-Tandem Mass Spectrometry（LC-MS-MS）, wherein GC and GC-MS methods poor anti jamming capability, pre-treatment
It is cumbersome.Contain multiple electronegativity groups in the structural formula of ethiprole and its metabolite, using gas chromatography tandem mass spectrometry method
（GC-MS-MS）In conjunction with negative chemical ionization source（NCI）With than electron impact ionization source（EI）It is preferably selective, it can significantly carry
High detection sensitivity allows using simple and efficient pre-treating method at possible.
Invention content
For overcome the deficiencies in the prior art, the present invention provides ethiprole in birds, beasts and eggs and its metabolite amide ethiproles
Gas Chromatography-Negative chemical source-tandem mass spectrum detection method.Due to bearing chemical source（NCI）Selectivity it is strong, detection sensitivity
It is significantly improved with the enhancing of testing molecule electronegativity, containing fluorine, chlorine atom in ethiprole and amide ethiprole structural formula, electricity is negative
Property is stronger, therefore selects NCI as ion source and have preferable selectivity, can significantly improve detection sensitivity.Tandem mass spectrum is because adopting
Use multiple-reaction monitoring（MRM）Pattern can be very good the background interference of removal complex matrices, realize the quantitative analysis to object.
Compared with current blanket monopole mass spectrum, there is stronger anti-matrix interference ability and qualitative, quantitative accuracy.This method
Chemical source-tandem mass spectrometry is born in conjunction with organophosphorous pesticides-, it can be to the ethiprole and its hydrolysate acyl in birds, beasts and eggs
Amine ethiprole is carried out at the same time measurement, and accurate, quick, high sensitivity that this method has the advantages that, is birds, beasts and eggs ethiprole and its metabolism
The remaining quick detection of product amide ethiprole provides reliable detection method and supports.
The present invention provides the Gas Chromatography-Negative chemical source-of ethiprole and its metabolite amide ethiprole in a kind of birds, beasts and eggs
Tandem mass spectrum detection method, includes the following steps：
（One）The extraction of sample to be tested：5.0-10.0g birds, beasts and eggs samples are weighed, extractant is then added and centrifuges speed in 15000r/min
The lower homogeneous of degree extracts 1min, and adding packet of saltouing shakes vigorously and mix well, and it is clear that upper layer is extracted after 10000r/min high speed centrifugations
Extractant is added in residual solution and repeats appeal step and merges gained clear liquid, gained clear liquid is placed in 40 DEG C of water again for liquid
It is concentrated under reduced pressure in bath until drying, is eventually adding the redissolution of 1.0-2.0mL extractants, obtains liquid to be clean；
（Two）The purification of liquid to be clean：Take step（One）In 1mL liquid to be clean be added to matrix dispersion purification pipe, vortex mixing
1min, the high speed centrifugation under 10000r/min speed take supernatant to obtain testing sample solution after 0.22 μm of membrane filtration；
（Three）The preparation of standard solution：Prepare ethiprole and amide ethiprole standard working solution, the standard working solution it is dense
It is respectively 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL, 50.0ng/mL, 100.0ng/ to spend gradient
ML, and it is added a concentration of 20.0 ng/mL's in each standard working solution13C2,15N2Ethiprole is formed mixed as internal standard compound
Standardization working solution；
（Four）The detection of testing sample solution：By step（Three）In testing sample solution and hybrid standard working solution in gas phase
Chromatography-, which is born, distinguishes sample introduction on chemical source-tandem mass spectrometer, obtain with a concentration of abscissa of object in standard solution, then with
The peak area of object is the working curve of ordinate in hybrid standard working solution, and each of parent ion can be determined by also obtaining
The first mass spectrometric figure of kind object after determining parent ion, is scanned using daughter ion and obtains second order ms figure, then from second order ms
Quota ion and qualitative ion are chosen in figure, and quantitative calculating, ethiprole and amide then are carried out to quota ion with working curve
Ethiprole with13C2,15N2Ethiprole is that internal standard uses inner mark method ration, obtains the concentration of object in testing sample solution.
The present invention is further arranged to the step（One）In Extraction solvent be acetonitrile.
The present invention is further arranged to the step（Two）In matrix dispersion purification pipe be WEL-QC-1202 type matrix point
Dissipate purification pipe.
The present invention is further arranged to the step（Four）The detection parameters of middle gas chromatography tandem mass spectrometry instrument are：
Chromatographic column：HP-5MS, 30m × 0.25mm × 0.25 μm；
Temperature programming：1min is kept at 60 DEG C, is heated up to 200 DEG C using the speed of 30 DEG C/min, then using 15 DEG C/min's
Speed is warming up to 300 DEG C, and keeps 5min；
Sample size：1μL；
Carrier gas：High-purity helium, purity >=99.999%, flow 1.0mL/min；
Collision gas：High-purity argon gas, purity >=99.999%；
Sample size mouth temperature：240℃；
Ion source：Chemical source negative ion mode（NCI）；Methane makees reaction gas, purity >=99.999%, flow 1.0mL/min；Source
Temperature：200℃.
Interface temperature：250℃；
Scan pattern：MRM patterns, ion pair and collision energy are as shown in the table：
The advantageous effect being arranged in this way is：Using the above scheme, first, the present invention is using remaining fluorine worm in acetonitrile extraction birds, beasts and eggs
Nitrile and amide ethiprole are added the buffer salt containing half times of magnesium sulfate, sodium citrate, sodium citrate hydrate and remove after extraction
Moisture and the rate of recovery for ensureing object.
Secondly, the present invention first uses the distribution of n-hexane liquid liquid to remove the fat in birds, beasts and eggs, then using containing magnesium sulfate, C18And PSA
The matrix dispersion purification pipe of material powder purifies sample liquid, can greatly impurity contained in birds, beasts and eggs, the suction without causing object
Loss is echoed, can guarantee the preferable rate of recovery.
Again, the present invention uses isotope standard inner mark method ration, can be imitated to the matrix on the pre-treatment rate of recovery and instrument
It should be corrected, ensure the accuracy of quantitative result.
Finally, Gas Chromatography-Negative chemical source of the present invention-tandem mass spectrum detector (GC-NCI-MS/MS) technology.Chemical-electrical
It is a kind of Soft ionization techniques from source, there is selectivity to the substance containing the electronegativity group such as fluorine, chlorine, nitro, in of the invention
Containing fluorine, cl radical in ethiprole and its hydrolysate amide ethiprole molecular structure, utilized using GC-NCI-MS/MS technologies
The high sensitivity combination NCI's of MS/MS is highly selective, greatly improves detection sensitivity so that sample purification process can
To take more fast and convenient method.
Description of the drawings
Fig. 1 is the chemical structural formula of ethiprole in the embodiment of the present invention；
Fig. 2 is the chemical structural formula of amide ethiprole in the embodiment of the present invention；
Fig. 3 is in the embodiment of the present invention13C2,15N2The chemical structural formula of ethiprole；
Fig. 4 is ethiprole in the embodiment of the present invention（2.0 ng/mL）MRM spectrograms；
Fig. 5 is amide ethiprole in the embodiment of the present invention（2.0 ng/mL）MRM spectrograms；
Fig. 6 is in the embodiment of the present invention13C2,15N2Ethiprole（20 ng/mL）MRM spectrograms；
Fig. 7 is the scanning second order ms figure of ethiprole in the embodiment of the present invention；
Fig. 8 is the scanning second order ms figure of amide ethiprole in the embodiment of the present invention；
Fig. 9 is in the embodiment of the present invention13C2,15N2The scanning second order ms figure of ethiprole；
Figure 10 is mark-on in egg sample in the embodiment of the present invention（2.0mg/kg）TLC spectrograms；
Figure 11 is the standard working curve of ethiprole in the embodiment of the present invention；
Figure 12 is the standard working curve of amide ethiprole in the embodiment of the present invention.
Specific implementation mode
The invention discloses ethiprole in a kind of birds, beasts and eggs and its metabolite amide fluorine worms it can be seen from Fig. 1 to Figure 12
Gas Chromatography-Negative chemical source-tandem mass spectrum detection method of nitrile, includes the following steps：
（One）The extraction of sample to be tested：5.0-10.0g birds, beasts and eggs samples are weighed, 10mL acetonitriles are then added and are centrifuged in 15000r/min
Homogeneous extracts 1min under speed, adds QuEChERS packets of saltouing and shakes vigorously and mix well, after 10000r/min high speed centrifugations
Supernatant liquor is extracted, extractant is added again in residual solution and repeats appeal step and merges gained clear liquid, by gained clear liquid
It is placed in 40 DEG C of water-baths and is concentrated under reduced pressure until drying, is eventually adding the redissolution of 1.0-2.0mL acetonitriles, obtains liquid to be clean；
（Two）The purification of liquid to be clean：Take step（One）In 1mL liquid to be clean be added to QuEChERS matrix dispersion purification pipe,
Vortex mixing 1min, the high speed centrifugation under 10000r/min speed take supernatant to be obtained after 0.22 μm of membrane filtration to be measured
Sample solution；
（Three）The preparation of standard solution：Prepare ethiprole and amide ethiprole standard working solution, the standard working solution it is dense
It is respectively 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL, 50.0ng/mL, 100.0ng/ to spend gradient
ML, and it is added a concentration of 20.0 ng/mL's in each standard working solution13C2,15N2Ethiprole is formed mixed as internal standard compound
Standardization working solution；
（Four）The detection of testing sample solution：By step（Three）In testing sample solution and hybrid standard working solution in gas phase
Chromatography-, which is born, distinguishes sample introduction on chemical source-tandem mass spectrometer, obtain with a concentration of abscissa of object in standard solution, then with
The peak area of object is the working curve of ordinate in hybrid standard working solution, and each of parent ion can be determined by also obtaining
The first mass spectrometric figure of kind object after determining parent ion, is scanned using daughter ion and obtains second order ms figure, then from second order ms
Quota ion and qualitative ion are chosen in figure, and quantitative calculating, ethiprole and amide then are carried out to quota ion with working curve
Ethiprole with13C2,15N2Ethiprole is that internal standard uses inner mark method ration, obtains the concentration of object in testing sample solution.
For the GC-NCI-MS/MS conditions of ethiprole in the embodiment of the present invention and amide ethiprole and its Isotopic Internal Standard, such as
Shown in following table：
*MS/MS quota ion pairs
The GC-NCI-MS/MS testing conditions of 1 each compound of table
For linear equation, related coefficient and the quantitative limit of 2 kinds of substances of ethiprole in the embodiment of the present invention and amide ethiprole, under entering
Shown in table：
| Compound | Linear equation | Related coefficient | Quantitative limit ng/g |
| Ethiprole | Y=0.02224X+0.03549 | 0.9991 | 0.2 |
| Amide ethiprole | Y=0.05355X+0.06393 | 0.9986 | 1.0 |
The linear equation of 2 each compound of table, related coefficient, quantitative limit
For the TIANZHU XINGNAO Capsul and precision of 2 kinds of substances of ethiprole in the embodiment of the present invention and amide ethiprole, as shown in the table：
Various concentration TIANZHU XINGNAO Capsul, precision (n=6) in 3 egg of table
The present invention is not limited to above-mentioned specific implementation mode, and persons skilled in the art according to the present disclosure, can
To implement of the invention or every design structure using the present invention and thinking using other a variety of specific implementation modes, do
Simple change or change, both fall within protection scope of the present invention.
Claims (4)
1. the Gas Chromatography-Negative chemical source of ethiprole and its metabolite amide ethiprole-tandem mass spectrum detection in a kind of birds, beasts and eggs
Method, it is characterised in that：Include the following steps：
The extraction of sample to be tested：5.0-10.0g birds, beasts and eggs samples are weighed, extractant is then added under 15000r/min centrifugal speeds
Homogeneous extracts 1min, adds packet of saltouing and shakes vigorously and mix well, supernatant liquor is extracted after 10000r/min high speed centrifugations,
Extractant is added in residual solution again to repeat appeal step and merge gained clear liquid, gained clear liquid is placed in 40 DEG C of water-baths and is subtracted
Pressure concentration is eventually adding the redissolution of 1.0-2.0mL extractants, obtains liquid to be clean until drying；
The purification of liquid to be clean：Take step（One）In 1mL liquid to be clean be added to matrix dispersion purification pipe, vortex mixing
1min, the high speed centrifugation under 10000r/min speed take supernatant to obtain testing sample solution after 0.22 μm of membrane filtration；
The preparation of standard solution：Prepare ethiprole and amide ethiprole standard working solution, the standard working solution concentration gradient
Respectively 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL, 20.0ng/mL, 50.0ng/mL, 100.0ng/mL, and
It is added a concentration of 20.0 ng/mL's in each standard working solution13C2,15N2Ethiprole forms hybrid standard as internal standard compound
Working solution；
The detection of testing sample solution：By step（Three）In testing sample solution and hybrid standard working solution in gas phase color
Distinguish sample introduction on the negative chemical source-tandem mass spectrometer of spectrum-, obtains with a concentration of abscissa of object in standard solution, then with mixed
The peak area of object is the working curve of ordinate in standardization working solution, and the various of parent ion can be determined by also obtaining
The first mass spectrometric figure of object after determining parent ion, is scanned using daughter ion and obtains second order ms figure, then from second order ms figure
Then middle selection quota ion and qualitative ion carry out quantitative calculating, ethiprole and amide fluorine with working curve to quota ion
Worm nitrile with13C2,15N2Ethiprole is that internal standard uses inner mark method ration, obtains the concentration of object in testing sample solution.
2. the Gas Chromatography-Negative of ethiprole and its metabolite amide ethiprole in a kind of birds, beasts and eggs according to claim 1
Chemical source-tandem mass spectrum detection method, it is characterised in that：The step（One）In Extraction solvent be acetonitrile.
3. the Gas Chromatography-Negative of ethiprole and its metabolite amide ethiprole in a kind of birds, beasts and eggs according to claim 1
Chemical source-tandem mass spectrum detection method, it is characterised in that：The step（Two）In matrix dispersion purification pipe be WEL-QC-
1202 type matrix dispersion purification pipe.
4. according to the Gas Chromatography-Negative chemical source-of ethiprole and its metabolite amide ethiprole in a kind of birds, beasts and eggs of claim 1
Tandem mass spectrum detection method, it is characterised in that：The step（Four）The detection parameters of middle gas chromatography tandem mass spectrometry instrument are：
Chromatographic column：HP-5MS, 30m × 0.25mm × 0.25 μm；
Temperature programming：1min is kept at 60 DEG C, is heated up to 200 DEG C using the speed of 30 DEG C/min, then using 15 DEG C/min's
Speed is warming up to 300 DEG C, and keeps 5min；
Sample size：1μL；
Carrier gas：High-purity helium, purity >=99.999%, flow 1.0mL/min；
Collision gas：High-purity argon gas, purity >=99.999%；
Sample size mouth temperature：240℃；
Ion source：Chemical source negative ion mode（NCI）；Methane makees reaction gas, purity >=99.999%, flow 1.0mL/min；Source
Temperature：200℃；
Interface temperature：250℃；
Scan pattern：MRM patterns, ion pair and collision energy are as follows, ethiprole, parent ion 366m/z, daughter ion 250,
318m/z, collision voltage 10,6eV；13C2,15N2Ethiprole, parent ion 370m/z, daughter ion 252,322m/z, collision voltage
It is 10,6eV；Amide ethiprole, parent ion 409.9m/z, daughter ion 253,339.9m/z, collision voltage 18,6eV.
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| CN115406994A (en) * | 2022-09-05 | 2022-11-29 | 广东省农业科学院植物保护研究所 | Method for measuring spodoptera frugiperda pesticide content by ultra-high performance liquid chromatography tandem mass spectrometry |
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