CN113219089A - Method for detecting urea by post-column derivatization-liquid chromatography - Google Patents
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Abstract
The invention provides a method for detecting urea by post-column derivatization-liquid chromatography, belonging to the technical field of detection. The method comprises the following steps: (1) taking a water sample to be detected, and injecting the water sample into a liquid chromatographic column for separation; (2) the mobile phase separated by the liquid chromatogram enters a derivatization pool and reacts with a derivatization reagent; (3) and (4) flowing the derivatized mobile phase into a fluorescence detector for fluorescence detection to obtain the urea content in the water sample to be detected. The method adopts a post-column derivatization liquid chromatography detection mode, urea is separated in a chromatographic column and then reacts with a derivatization reagent in a derivatization tank, and the method has the advantages of high sensitivity, low detection limit and strong anti-interference capability.
Description
Technical Field
The invention belongs to the field of chemical analysis, and particularly relates to a method for detecting urea by post-column derivatization-liquid chromatography.
Background
Urea that human metabolism decomposes protein in-process production can be along with urine, sweat discharge extracorporeally, and the extrasomatic urea of these discharges can cause the pollution to the water when the people is swimming, can cause multiple disease even when urea concentration exceeds standard, more probably causes the damage to the skin mucous membrane. The urea content in the swimming pool water is used as an important index for public health monitoring, which reflects the pollution condition of the swimming pool water, and the mass concentration of the urea in the swimming pool water must be less than 3.5mg/L according to the public place health index and limit value requirements of GB 37488-one 2019 formulated by the State market supervision and administration Bureau. Therefore, it is necessary to detect urea in water.
At present, methods for detecting the content of urea in water comprise a spectrophotometric method, a flow injection spectrophotometric method, a urease-glutamate dehydrogenase coupling rate determination method and a pre-column derivatization-liquid chromatography fluorescence detection method, however, the methods have the defects of long pretreatment time, poor water bath heating color development stability, poor linearity, narrow linear range, difficult separation of pre-column derivatization byproducts, easy introduction of impurities in the pre-column derivatization process and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for detecting urea by post-column derivatization-liquid chromatography. The method for detecting urea by post-column derivatization-liquid chromatography adopts post-column derivatization, and has the advantages of high sensitivity, low detection limit and strong anti-interference capability.
In order to achieve the purpose, a method for detecting urea by post-column derivatization-liquid chromatography is adopted, and comprises the following steps:
(1) taking a water sample to be detected, and injecting the water sample into a liquid chromatographic column for separation;
(2) the mobile phase separated by the liquid chromatogram enters a derivatization pool and reacts with a derivatization reagent;
(3) and (4) flowing the derivatized mobile phase into a fluorescence detector for fluorescence detection to obtain the urea content in the water sample to be detected.
According to the method for detecting the urea by the post-column derivatization-liquid chromatography, the urea is separated in the chromatographic column and then reacts with a derivatization reagent in a derivatization pool, and a derivatization product is detected. The sensor has the advantages of high sensitivity, low detection limit and strong anti-interference capability due to the good reproducibility, few influence factors and few introduced substances.
In one embodiment, the column is an HSS T3 column. Urea as a strongly polar compound, conventional general-purpose reversed phase C18The column is only suitable for analyzing nonpolar or neutral compounds, strong polar compounds are not retained, and the compatibility with water phase is not good, the inventor selects an HSS T3 chromatographic column to separate urea after repeated screening and comparison, and the HSS T3 chromatographic column has stronger reversed phase retention capacity to polar molecules and has better effect on the retention of urea on the column.
In one embodiment, the column size is 150mm by 4.6mm, and the packing particle size is 5 μm.
In one embodiment, the derivatizing agent is 0.5 + -0.2 g/L of xanthene hydro-alcohol methanol aqueous solution containing 0.5 + -0.2% by volume of hydrochloric acid.
It will be understood that the above volume percent concentrations are based on 100% concentrated hydrochloric acid (12mol/L), i.e. 0.5% by volume hydrochloric acid means 0.5mL of concentrated hydrochloric acid in 100mL of solution.
In the conventional technology, urease and iodine are usually selected as post-column derivatization reagents of urea, and determination is carried out through multi-step reaction, but the operation is complicated, and xanthene hydro-alcohol is adopted as a derivatization reagent, so that the determination steps can be simplified.
In one embodiment, the volume ratio of methanol to water in the derivatizing reagent is 3 ± 0.5: 1. Xanthene hydro-alcohol is insoluble in water and soluble in alcohol, and is easy to cause system pressure overpressure, so that the application of the xanthene hydro-alcohol in post-column derivatization is greatly limited. According to the invention, the xanthene hydro-alcohol derivatization reagent is prepared by adopting the mixed solvent of methanol and water, and the ratio of an organic phase to a water phase is repeatedly tried to be adjusted, so that the problem of system pressure overpressure caused by water insolubility is successfully solved, and the xanthene hydro-alcohol can be used for post-column derivatization detection.
In one embodiment, the derivatizing agent is formulated by: weighing 0.50 +/-0.2 g of xanthene hydro-alcohol, dissolving in 750mL of methanol, adding 250mL of deionized water, adding 5 +/-2 mL of concentrated hydrochloric acid, adding methanol to reach the constant volume of 1000mL, and carrying out vacuum filtration to obtain the xanthene hydro-alcohol.
In the prior art, xanthene hydro-alcohol is adopted to detect urea in pre-column derivatization, and the derivatization reagent enables the xanthene hydro-alcohol to be successfully applied to a method for detecting urea by post-column derivatization-liquid chromatography, and a fluorescent substance is not required to be generated by means of multi-step post-column derivatization reaction of enzyme or iodine for determination.
In one embodiment, the liquid chromatography separation uses isocratic elution, and the elution conditions include:
column temperature: 40 +/-5 ℃;
mobile phase: deionized water;
flow rate: 0.75 plus or minus 0.1 mL/min.
The isocratic elution mode avoids using a complex mobile phase system.
In one embodiment the temperature of the derivatization cell is 35-50 deg.C and the flow rate of the derivatizing agent into the derivatization cell is 0.25. + -. 0.05 mL/min. By adopting the conditions, on-line derivatization can be realized, so that the peak area generated by urea derivatization is maximum.
In one embodiment, the fluorescence detector has an excitation wavelength of 213. + -.2 nm and an emission wavelength of 308. + -.2 nm. In the prior art, two fluorescence detection wavelengths are available for xanthene hydro-alcohol and urea pre-column derivative products, wherein one excitation wavelength is 233nm, and the emission wavelength is 600 nm; and the other excitation wavelength is 213nm and the emission wavelength is 308nm, and the mobile phase is derived by comparing the two wavelengths of 3D scanning urea standard solution, so that the base line is stable and the noise is low when the excitation wavelength is 213nm and the emission wavelength is 308 nm.
In the method, the retention time of the standard derivative of a reference substance solution is used for qualitative determination, and the standard method is used for quantitative determination.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for detecting urea by post-column derivatization-liquid chromatography, a post-column derivatization liquid chromatography detection mode is adopted, urea is separated in a chromatographic column and then reacts with a derivatization reagent in a derivatization pool, and the method has the advantages of high sensitivity, low detection limit and strong anti-interference capability.
In addition, the method avoids using a complex mobile phase system, does not need to generate a fluorescent substance for determination by means of enzyme or iodine multi-step post-column derivatization reaction, and solves the problems of long pretreatment time, poor water-bath heating color development stability, poor linearity, narrow linear range and the like of the national standard spectrophotometry. Experimental results show that the method for determining urea in water has the advantages that the mass concentration of urea is in good linearity within the range of 1.0-100.0 mg/L, the correlation coefficient is 0.9999, the detection limit of the method is 0.18mg/L, the quantification limit is 0.54mg/L, the standard recovery rate is 91.7-103.4%, the RSD is 1.2-4.7%, and the method has good detection performance.
Drawings
FIG. 1 is a graph showing the effect of different derivatization pool temperatures on the peak area of urea-derived products in example 2 of the present invention;
FIG. 2 is a chromatogram of a standard derivative of urea according to example 4 of the present invention;
FIG. 3 is a chromatogram of a standard solution of 250mg/L ammonia and 100mg/L urea in example 4 of the present invention;
FIG. 4 is a 100mg/L total ion chromatogram of a urea derivative in electrospray positive ion mode in example 3 of the present invention;
FIG. 5 is a structural diagram of the product N, N-diureido xanthene derived from the urea standard in example 3 of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings and examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Defining:
the HSS T3 chromatographic column is a C18 chromatographic column which is compatible with 100% aqueous mobile phase and adopts high-strength silica gel (TSS) as a matrix.
Materials, reagents, instruments, sources of statistical analysis software to which the following examples refer:
materials: the water samples to be tested are derived from tap water, swimming pool water and river surge water in the district of Cambodia city, Guangzhou.
Reagent: the standard substance GBW09201 of urea purity is from China institute of metrology science, purity>99.8 percent; the xanthene hydro-alcohol is purchased from Shanghai Aladdin Biotechnology, Inc., with a purity of 98%; methanol was purchased from Shanghai' an spectra experiment science and technology, Inc., UV-HPLC grade; the hydrochloric acid is purchased from Guangzhou chemical reagent factories and is of high-grade purity; the trichloromethane is purchased from Guangzhou chemical reagent factories and is analyzed and purified; the experimental water is deionized water, and the resistance value is 18.3M omega cm-2(ii) a 0.20 μm GHP cartridges were purchased from Waters, USA.
The instrument adopts: waters
A T3 chromatography column; a us Waters e2695 high performance liquid chromatograph equipped with 2475 fluorescence detector, empower3.0 chromatography workstation; us PICKERING PINNACLE PCX post-column derivitizer; a METTLER TOLEDO XS205DU electronic balance, switzerland; bruker Daltonic GmbH Bremn fourier transform ion cyclotron resonance mass spectrometer, germany; tianjin GM-0.50 Jinteng diaphragm vacuum pump; kunshan KQ5200DB model digital control ultrasonic cleaner.
Statistical analysis software: data processing and mapping were performed using Microsoft Excel 2010 and Origin Pro 8.0.
Reagents and materials used in the present example are all commercially available sources unless otherwise specified; unless otherwise specified, all the experimental methods are routine in the art.
Example 1
A method for detecting urea by post-column derivatization-liquid chromatography comprises the following steps:
1. a water sample to be detected is taken and injected into a liquid chromatographic column for separation, and the method specifically comprises the following steps:
taking a water sample, directly feeding the sample after passing through a 0.20 mu m GHP filter head, and carrying out liquid chromatography separation.
Wherein, the liquid phase conditions are as follows:
a chromatographic column: waters
T3(150mm×4.6mm，5μm)；
Column temperature: 40 ℃;
mobile phase: deionized water, isocratic elution, flow rate: 0.75 mL/min;
the injection volume was 100. mu.L.
2. The mobile phase separated by the liquid chromatogram enters a derivatization pool and reacts with a derivatization reagent, and the specific conditions are as follows:
volume of the derivatization pool: 1.4 mL;
temperature: 40 ℃;
derivatization reagent: 0.5% hydrochloric acid in 0.5g/L xanthenehydronol methanol aqueous solution (methanol: water ═ 3:1, V/V);
flow rate of derivatizing reagent: 0.25 mL/min.
3. And (3) flowing the derivatized mobile phase into a fluorescence detector for fluorescence detection to obtain the urea content in the water sample to be detected, wherein the method specifically comprises the following steps:
the detector is a fluorescence detector: the excitation wavelength is 213nm, and the emission wavelength is 308 nm;
the retention time is used for qualitative determination, and the peak area external standard method is used for quantitative determination.
The preparation method of the standard solution and the standard series comprises the following steps:
accurately weighing 0.1000g of urea purity standard substance in a small beaker, adding a small amount of deionized water to dissolve the substance, transferring the substance into a 100mL volumetric flask, adding 1mL of trichloromethane, and fixing the volume with the deionized water to obtain 1000mg/L urea standard stock solution. Storing at 4 deg.C for 30 days. Diluting 100.0mg/L urea standard stock solution with deionized water step by step to prepare 1.0, 2.5, 5.0, 10.0, 20.0, 50.0 and 100.0mg/L standard series solutions respectively.
4. Calculation of results
And (4) finding out the mass concentration (mg/L) of the urea from the standard curve according to the peak height or peak area of the water sample, namely the urea content in the water sample. Wherein statistical analysis was performed using Microsoft Excel 2010 and Origin Pro 8.0 for data processing and mapping.
Example 2
And (4) screening the temperature of the derivatization pool.
This example was run with a 20mg/L urea standard solution, operating under the same conditions as example 1, except that:
the temperature of the derivation pool is between 30 ℃ and 100 ℃.
The situation of derivatization reaction is shown in figure 1, and the result shows that when the reaction temperature reaches 40 ℃, the peak area of the urea derivative product is the largest, and the reaction is an exothermic reaction through analysis, and the temperature is increased to be unfavorable for the derivatization reaction, so that the temperature of 40 ℃ is used as the temperature of a derivatization pool.
Example 3
And (4) determination of derivative products.
The inventors speculated from the molecular structural formulae of urea and xanthene hydro-alcohol that there may be 2 derivative products: 9-ureidoxanthene (N-9H-xanthen-9-yl) and N, N-diureidene (N, N-di-9H-xanthem-9-yl) have relative molecular masses of 240 and 420, respectively.
Further, the post-column derived product with retention time of 100mg/L urea standard solution between 3.8min and 4.8min was collected and subjected to full scan by an electrospray positive ion mode Fourier transform ion cyclotron resonance mass spectrometer and found to be at M/z 421([ M + H ])]+) There is a distinct peak (as shown in FIG. 4), and M/z 241([ M + H)]+) There is no significant signal response. Therefore, it is concluded that under the derivatization conditions, the derivative product of the urea standard is N, N-di-9H-xanthem-9-yl urea (shown in FIG. 5).
Example 4
And (5) verifying the methodology.
1. Chromatographic separation and interference test
The chromatographic separation and the interferences were examined with a 20mg/L urea standard solution according to the experimental conditions of example 1.
1.1 Experimental methods.
Sucking 1.00mL of 1000mg/L urea standard stock solution into a 10mL volumetric flask, transferring 5.00mL of 500mg/L ammonia standard solution into the volumetric flask, fixing the volume to a scale mark by using deionized water to obtain a mixed solution of 250mg/L ammonia and 100mg/L urea, and treating the mixed solution according to the experimental conditions of the embodiment 1.
1.2 the results of the experiment.
The post-column derivatization separation is shown in FIG. 2, with a retention time of 4.11min, where it can be seen that there is no interference of reactants and reaction by-products before and after the target retention time. Also, 250mg/L ammonia did not interfere with the measurement of 100mg/L urea, as shown in FIG. 3.
2. Linearity, detection limit and quantification limit of the method
The standard solutions prepared in example 1 were subjected to on-machine measurement under the chromatographic conditions in example 1, and the urea standard solutions were well-linear in the range of 1.0mg/L to 100.0mg/L, and the regression equation was-1.93X 10 ═ Y4+1.17×105X (X: concentration, Y: peak area) and correlation coefficient r ═ 0.9999.
According to the 3-time signal-to-noise ratio (S/N), the detection limit of the method is calculated to be 0.18mg/L, and the quantification limit of the method is measured to be 0.54mg/L through experiments.
3. Method for adding standard and recovering and testing precision
The tap water is adopted to simulate urea samples with high, medium and low concentration levels to carry out standard addition recovery and precision tests, urea standard solutions with high, medium and low concentration levels are added into the samples to be processed and analyzed according to the method in the example 1, the standard addition recovery rate and the RSD (n is 6) result are calculated after 6 times of parallel measurement, and the standard addition recovery rate of the urea and the RSD (n is 6) result are shown in the following table, so that the standard addition recovery rate of the urea is 91.7-103.4% and the RSD is 1.2-4.7%.
TABLE 1 standard urea recovery test and precision test (n ═ 6)
4. Preservation and analysis of water samples
The urea sample with different concentration levels is stored at 4 ℃ in a refrigeration mode, the stability of the sample solution is respectively measured, the results are shown in the table, and the table shows that the urea sample solution is relatively stable within 14 days under the refrigeration storage at 4 ℃.
TABLE 2 stability test of urea sample solutions at 4 ℃ in cold storage
Example 5
For 1 part of tap water, 1 part of river surge water and 2 parts of swimming pool water in the jurisdiction of Cambodia, 4 parts of water samples are respectively detected according to the steps of example 1. And (3) detecting results, wherein the water samples of the tap water, the river water and 1 part of swimming pool water are less than the detection limit, and the urea content of the other 1 part of swimming pool water is 2.76 mg/L.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for detecting urea by post-column derivatization-liquid chromatography is characterized by comprising the following steps:
(1) taking a water sample to be detected, and injecting the water sample into a liquid chromatographic column for separation;
(2) the mobile phase separated by the liquid chromatogram enters a derivatization pool and reacts with a derivatization reagent;
(3) and (4) flowing the derivatized mobile phase into a fluorescence detector for fluorescence detection to obtain the urea content in the water sample to be detected.
2. The method of claim 1, wherein the chromatography column is an HSS T3 chromatography column.
3. The method of claim 2, wherein the column size is 150mm x 4.6mm and the packing particle size is 5 μm.
4. The method of claim 1 wherein said derivatizing agent is 0.5 + 0.2g/L of an aqueous solution of xanthene hydro-alcohol in methanol with a concentration of 0.5 + 0.2% by volume of hydrochloric acid.
5. The method of claim 4, wherein the volume ratio of methanol to water in the derivatizing reagent is 3 ± 0.5: 1.
6. The method of claim 5, wherein the derivatizing agent is formulated by:
weighing 0.50 +/-0.2 g of xanthene hydro-alcohol, dissolving in 750mL of methanol, adding 250mL of deionized water, adding 5 +/-2 mL of concentrated hydrochloric acid, adding methanol to reach the constant volume of 1000mL, and carrying out vacuum filtration to obtain the xanthene hydro-alcohol.
7. The method of claim 1, wherein the liquid chromatography is performed using isocratic elution under conditions comprising:
column temperature: 40 +/-5 ℃;
mobile phase: deionized water;
flow rate: 0.75 plus or minus 0.1 mL/min.
8. The method of claim 7, wherein the temperature of the derivatization cell is 35-50 ℃ and the flow rate of the derivatizing agent into the derivatization cell is 0.25 ± 0.05 mL/min.
9. The method of claim 1, wherein the fluorescence detector has an excitation wavelength of 213 ± 2nm and an emission wavelength of 308 ± 2 nm.
10. The method of claim 1, wherein the standard derivative retention time of the reference solution is qualitative and the external standard is quantitative.
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