CN117783392A - Method for detecting free glucosamine in pesticide plant protection product - Google Patents
Method for detecting free glucosamine in pesticide plant protection product Download PDFInfo
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- CN117783392A CN117783392A CN202311860581.1A CN202311860581A CN117783392A CN 117783392 A CN117783392 A CN 117783392A CN 202311860581 A CN202311860581 A CN 202311860581A CN 117783392 A CN117783392 A CN 117783392A
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- plant protection
- glucosamine
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- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 title claims abstract description 29
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229960002442 glucosamine Drugs 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000000575 pesticide Substances 0.000 title claims abstract description 17
- 239000004476 plant protection product Substances 0.000 title claims abstract description 17
- 239000012488 sample solution Substances 0.000 claims abstract description 37
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims abstract description 9
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims abstract description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 3
- 239000000945 filler Substances 0.000 claims abstract description 3
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 3
- 239000010935 stainless steel Substances 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 18
- 238000007865 diluting Methods 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 229910021538 borax Inorganic materials 0.000 claims description 9
- 239000007853 buffer solution Substances 0.000 claims description 9
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 9
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 239000012085 test solution Substances 0.000 claims description 7
- CBOJBBMQJBVCMW-BTVCFUMJSA-N (2r,3r,4s,5r)-2-amino-3,4,5,6-tetrahydroxyhexanal;hydrochloride Chemical compound Cl.O=C[C@H](N)[C@@H](O)[C@H](O)[C@H](O)CO CBOJBBMQJBVCMW-BTVCFUMJSA-N 0.000 claims description 6
- 229960001911 glucosamine hydrochloride Drugs 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004811 liquid chromatography Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 125000003396 thiol group Chemical group [H]S* 0.000 abstract description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 230000009257 reactivity Effects 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 2
- -1 sulfhydryl ethanol Chemical compound 0.000 abstract description 2
- 238000001212 derivatisation Methods 0.000 description 11
- ZWLUXSQADUDCSB-UHFFFAOYSA-N phthalaldehyde Chemical compound O=CC1=CC=CC=C1C=O ZWLUXSQADUDCSB-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012483 derivatization solution Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002301 glucosamine derivatives Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the technical field of detection, and particularly relates to a method for detecting free glucosamine in pesticide plant protection products, which comprises the steps of taking methanol, acetonitrile and 0.04% phosphoric acid water as mobile phases, using a stainless steel column with C18 as a filler and an ultraviolet detector, mixing a sample solution with a derivative solution in air, performing high performance liquid chromatography separation and determination, and quantitatively using a chromatographic column as an external standard, wherein the derivative solution contains mercaptoethanol. The invention solves the problems of long reaction, high temperature and poor stability of the existing derivative, utilizes the hydroxyl group and the sulfhydryl group on the sulfhydryl ethanol to form effective connection, improves the reactivity of the sulfhydryl group, reduces the temperature of the derivative reaction, realizes normal-temperature reaction, and simultaneously can greatly improve the stability of the derivative.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for detecting free glucosamine in pesticide plant protection products.
Background
Glucosamine is a small molecular monosaccharide widely existing in nature, and has wide application in the fields of medicines, health products and the like. The current detection methods of glucosamine are mainly classified into spectrophotometry, ion chromatography and derivatization. However, in spectrophotometry, the derived product is unstable, and the color development gradually deepens with time, affecting the accuracy of the content; in addition, when the color of the sample exists, the interference can be seriously generated, so that the content of the glucosamine is seriously ultrahigh; ion chromatography separates glucosamine and other components in Henan when the sample components are complex; the derivatization method needs to be carried out in dark and light-proof conditions, and mercaptopropionic acid can introduce various side reactions in the reaction of glucosamine and phthalic aldehyde, so that the derivatization product is complex, and serious interference is generated on the measurement of the result.
Therefore, there is a need for a method for detecting glucosamine that has stable derivatization and good stability of derivatives.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for detecting free glucosamine in pesticide plant protection products, which solves the problems of long reaction, high temperature and poor stability of the existing derivatives, utilizes hydroxyl and sulfhydryl on mercaptoethanol to form effective connection, improves the reactivity of sulfhydryl, reduces the temperature of the derivative reaction, realizes normal-temperature reaction, and simultaneously can greatly improve the stability of the derivatives.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a method for detecting free glucosamine in pesticide plant protection products uses methanol, acetonitrile and 0.04% phosphoric acid water as mobile phases, a stainless steel column with C18 as a filler and an ultraviolet detector, and after air mixing a sample solution and a derivative solution, high performance liquid chromatography separation and determination are carried out, and an external standard method uses a chromatographic column quantitatively.
The derivative solution contains mercaptoethanol.
The flow rate of the liquid chromatography is 1mL/min, the column temperature is 30 ℃, and the temperature change is not more than 2 ℃.
The detection wavelength is 330nm.
The sample injection volume was 10. Mu.L.
The method comprises the following specific steps:
step 1, preparing a standard sample solution: weighing 0.01g of glucosamine hydrochloride standard sample, placing into a 50mL volumetric flask, diluting to scale with deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking to obtain solution A;
step 2, transferring 5mL of the solution A into a 50mL volumetric flask by using a pipette, diluting to a scale by using deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking uniformly to obtain a standard sample solution;
step 3, preparation of a sample solution: weighing 1g of a sample, placing the sample in a 50mL volumetric flask, diluting the sample to a scale with water, carrying out ultrasonic oscillation for 5min to completely dissolve the sample, cooling the sample to room temperature, and shaking the sample to obtain a sample solution;
step 4, preparation of derivative solution: 0.1g of OPA is weighed and dissolved by 10mL of methanol, 0.1g of mercaptoethanol and 0.4mol/L of sodium borate buffer solution are added to fix the volume to 100mL, and a derivative solution is obtained, wherein the sodium borate buffer solution is prepared by weighing 2.48g of boric acid and 1.41g of sodium hydroxide, and dissolving the solution with water to fix the volume to 100mL.
And 5, continuously injecting a plurality of needles of standard sample solution after the instrument is stable, calculating the relative response value of each needle, and measuring according to the sequence of the standard sample solution, the sample solution and the standard sample solution after the change of the glucosamine relative response values of two adjacent needles is less than 1.5%.
Before the measurement, the derivative solution is mixed with the test solution by an air bath, and after a few seconds, the mixture is injected into a liquid chromatograph.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problems of long reaction, high temperature and poor stability of the existing derivative, utilizes the hydroxyl group and the sulfhydryl group on the sulfhydryl ethanol to form effective connection, improves the reactivity of the sulfhydryl group, reduces the temperature of the derivative reaction, realizes normal-temperature reaction, and simultaneously can greatly improve the stability of the derivative.
2. According to the invention, through the active reaction of the mercaptoethanol, the normal-temperature rapid reaction of the glucosamine and the phthalic aldehyde is promoted, the time of the derivatization reaction is reduced, the feasibility of pre-column derivatization mixing is realized, and the problem of decomposition of a derivatization product in the time of placing to-be-detected is avoided.
Drawings
FIG. 1 is a liquid chromatogram of a glucosamine standard derivatization solution (mercaptoethanol as derivatizing agent).
Detailed Description
One embodiment of the present invention is described in detail with reference to fig. 1, but does not limit the claims of the present invention in any way.
Example 1
A method of detecting free glucosamine in pesticide plant protection products, comprising:
step 1, preparing a standard sample solution: weighing 0.01g of glucosamine hydrochloride standard sample, placing into a 50mL volumetric flask, diluting to scale with deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking to obtain solution A;
step 2, transferring 5mL of the solution A into a 50mL volumetric flask by using a pipette, diluting to a scale by using deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking uniformly to obtain a standard sample solution;
step 3, preparation of a sample solution: weighing 1g of a sample, placing the sample in a 50mL volumetric flask, diluting the sample to a scale with water, carrying out ultrasonic oscillation for 5min to completely dissolve the sample, cooling the sample to room temperature, and shaking the sample to obtain a sample solution;
step 4, preparation of derivative solution: 0.1g of OPA is weighed and dissolved by 10mL of methanol, 0.1g of mercaptoethanol and 0.4mol/L of sodium borate buffer solution are added to fix the volume to 100mL, and a derivative solution is obtained, wherein the sodium borate buffer solution is prepared by weighing 2.48g of boric acid and 1.41g of sodium hydroxide, and dissolving the solution with water to fix the volume to 100mL.
And 5, after the instrument is stabilized, carrying out liquid chromatography analysis on the standard sample solution and the sample solution, wherein before measurement, the derivative solution is mixed with the test solution through an air bath at normal temperature, and is injected into a liquid chromatograph after a few seconds, and the volume ratio of the derivative solution to the test solution is as follows: 1:1.
As shown in figure 1, the characteristic peak of the glucosamine derivative product is detected in 7-8min, the peak type is symmetrical, other interference-free miscellaneous peaks are avoided, and the separation degree and the selectivity are good.
Comparative example 1
A method of detecting free glucosamine in pesticide plant protection products, comprising:
step 1, preparing a standard sample solution: weighing 0.01g of glucosamine hydrochloride standard sample, placing into a 50mL volumetric flask, diluting to scale with deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking to obtain solution A;
step 2, transferring 5mL of the solution A into a 50mL volumetric flask by using a pipette, diluting to a scale by using deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking uniformly to obtain a standard sample solution;
step 3, preparation of a sample solution: weighing 1g of a sample, placing the sample in a 50mL volumetric flask, diluting the sample to a scale with water, carrying out ultrasonic oscillation for 5min to completely dissolve the sample, cooling the sample to room temperature, and shaking the sample to obtain a sample solution;
step 4, preparation of derivative solution: 0.1g of OPA is weighed and dissolved by 10mL of methanol, 0.1g of mercaptopropionic acid is added, the volume is fixed to 100mL of 0.4mol/L sodium borate buffer solution, and a derivative solution is obtained, 2.48g of boric acid and 1.41g of sodium hydroxide are weighed, and the solution is dissolved by water and the volume is fixed to 100mL.
Step 5, the derivative solution and the test solution are subjected to 1:1, and then placing the mixture in a dark place for 1min, and taking the reaction liquid for liquid phase analysis.
And 6, testing the derivative liquid in the step 5 after the instrument is stabilized.
Under this derivatization condition, almost no chromatographic peak of glucosamine and OPA-derivatized products was detected.
Comparative example 2
A method of detecting free glucosamine in pesticide plant protection products, comprising:
step 1, preparing a standard sample solution: weighing 0.01g of glucosamine hydrochloride standard sample, placing into a 50mL volumetric flask, diluting to scale with deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking to obtain solution A;
step 2, transferring 5mL of the solution A into a 50mL volumetric flask by using a pipette, diluting to a scale by using deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking uniformly to obtain a standard sample solution;
step 3, preparation of a sample solution: weighing 1g of a sample, placing the sample in a 50mL volumetric flask, diluting the sample to a scale with water, carrying out ultrasonic oscillation for 5min to completely dissolve the sample, cooling the sample to room temperature, and shaking the sample to obtain a sample solution;
step 4, preparation of derivative solution: 0.1g of OPA is weighed and dissolved by 10mL of methanol, 0.1g of mercaptopropionic acid is added, the volume is fixed to 100mL of 0.4mol/L sodium borate buffer solution, and a derivative solution is obtained, 2.48g of boric acid and 1.41g of sodium hydroxide are weighed, and the solution is dissolved by water and the volume is fixed to 100mL.
Step 5, the derivative solution and the test solution are subjected to 1:1, and then placing the mixture in a dark place for 10min, and taking the reaction liquid for liquid phase analysis.
And 6, after the instrument is stabilized, carrying out liquid chromatography analysis on the derivatization solution in the step 5.
Under this derivatization condition, chromatographic peaks of glucosamine and OPA-derivatized products can be detected.
Comparative example 3
A method of detecting free glucosamine in pesticide plant protection products, comprising:
step 1, preparing a standard sample solution: weighing 0.01g of glucosamine hydrochloride standard sample, placing into a 50mL volumetric flask, diluting to scale with deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking to obtain solution A;
step 2, transferring 5mL of the solution A into a 50mL volumetric flask by using a pipette, diluting to a scale by using deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking uniformly to obtain a standard sample solution;
step 3, preparation of a sample solution: weighing 1g of a sample, placing the sample in a 50mL volumetric flask, diluting the sample to a scale with water, carrying out ultrasonic oscillation for 5min to completely dissolve the sample, cooling the sample to room temperature, and shaking the sample to obtain a sample solution;
step 4, preparation of derivative solution: 0.1g of OPA is weighed and dissolved by 10mL of methanol, 0.1g of mercaptopropionic acid is added, the volume is fixed to 100mL of 0.4mol/L sodium borate buffer solution, and a derivative solution is obtained, 2.48g of boric acid and 1.41g of sodium hydroxide are weighed, and the solution is dissolved by water and the volume is fixed to 100mL.
Step 5, the derivative solution and the test solution are subjected to 1:1, standing for 30min under natural light, and then taking the reaction liquid for liquid phase analysis.
And 6, performing liquid chromatography analysis on the derivatization solution in the step 5.
Under the derivatization condition, a relatively impure chromatographic peak is detected in the chromatograph, and interference is formed on judgment and quantification of the derivatization products of the target components.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (7)
1. A method for detecting free glucosamine in pesticide plant protection products is characterized by comprising the following steps: the method uses methanol, acetonitrile and 0.04% phosphoric acid water as mobile phases, uses a stainless steel column with C18 as a filler and an ultraviolet detector, carries out air mixing on a sample solution and a derivative solution, carries out high performance liquid chromatography separation and determination, and quantitatively uses a chromatographic column by an external standard method; the derivative solution contains mercaptoethanol.
2. The method for detecting free glucosamine in pesticide plant protection products according to claim 1, wherein: the flow rate of the liquid chromatography is 1mL/min, the column temperature is 30 ℃, and the temperature change is not more than 2 ℃.
3. The method for detecting free glucosamine in pesticide plant protection products according to claim 1, wherein: the detection wavelength is 330nm.
4. The method for detecting free glucosamine in pesticide plant protection products according to claim 1, wherein: the sample injection volume was 10. Mu.L.
5. The method for detecting free glucosamine in pesticide plant protection products according to claim 1, wherein: the method comprises the following specific steps:
step 1, preparing a standard sample solution: weighing 0.01g of glucosamine hydrochloride standard sample, placing into a 50mL volumetric flask, diluting to scale with deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking to obtain solution A;
step 2, transferring 5mL of the solution A into a 50mL volumetric flask by using a pipette, diluting to a scale by using deionized water, ultrasonically oscillating for 5min, completely dissolving, cooling to room temperature, and shaking uniformly to obtain a standard sample solution;
step 3, preparation of a sample solution: weighing 1g of a sample, placing the sample in a 50mL volumetric flask, diluting the sample to a scale with water, carrying out ultrasonic oscillation for 5min to completely dissolve the sample, cooling the sample to room temperature, and shaking the sample to obtain a sample solution;
step 4, preparation of derivative solution: weighing 0.1g of OPA, dissolving with 10mL of methanol, adding 0.1g of mercaptoethanol, and fixing the volume of 0.4mol/L sodium borate buffer solution to 100mL to obtain a derivative solution;
and 5, continuously injecting a plurality of needles of standard sample solution after the instrument is stable, calculating the relative response value of each needle, and measuring according to the sequence of the standard sample solution, the sample solution and the standard sample solution after the change of the glucosamine relative response values of two adjacent needles is less than 1.5%.
6. The method for detecting free glucosamine in a pesticide plant protection product as set forth in claim 5, wherein: the determination in the step 5 is that the derivative solution is mixed with the test solution through an air bath, and the mixture is injected into a liquid chromatograph after a few seconds.
7. The method for detecting free glucosamine in a pesticide plant protection product as set forth in claim 5, wherein: the sodium borate buffer solution is prepared by weighing 2.48g of boric acid and 1.41g of sodium hydroxide, and dissolving the boric acid and the sodium hydroxide in water to constant volume to 100mL.
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| CN202311860581.1A CN117783392A (en) | 2023-12-31 | 2023-12-31 | Method for detecting free glucosamine in pesticide plant protection product |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311860581.1A CN117783392A (en) | 2023-12-31 | 2023-12-31 | Method for detecting free glucosamine in pesticide plant protection product |
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| CN202311860581.1A Pending CN117783392A (en) | 2023-12-31 | 2023-12-31 | Method for detecting free glucosamine in pesticide plant protection product |
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| CN (1) | CN117783392A (en) |
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