CN-121994948-A - Method for detecting p-nitroiodobenzene in water body and soil based on ultra-high performance liquid chromatography

CN121994948ACN 121994948 ACN121994948 ACN 121994948ACN-121994948-A

Abstract

The invention discloses a method for detecting p-nitroiodobenzene in water and soil based on ultra-high performance liquid chromatography, which comprises the following steps of firstly, detecting by using an ultra-high performance liquid chromatograph, and determining different detection conditions according to the water and the soil; the invention has the advantages that the retention time of the p-nitroiodobenzene in the water body is about 2.9 min, the target peak and other components can realize baseline separation under the detection wavelength of 296nm, other impurity interference phenomena are not generated, the method has good selectivity, the retention time of the p-nitroiodobenzene in the soil under the detection wavelength of 296nm is about 6.1 min, the target peak can realize baseline separation, the separation degree with other impurity peaks is more than 1.5, and the method has good selectivity.

Inventors

DONG RONGGUI
HUANG YONGHUI
An Xiaosi
ZHOU JING

Assignees

贵州健安德科技有限公司

Dates

Publication Date: 20260508
Application Date: 20251119

Claims (6)

1. The method for detecting p-nitroiodobenzene in water and soil based on ultra-high performance liquid chromatography is characterized by comprising the following steps of: Detecting by using an ultra-high performance liquid chromatograph, and determining different detection conditions according to water and soil; step two, preparing a working solution of the detected object, wherein the configuration comprises the configuration of a standard stock solution and the configuration of the standard working solution; The specificity experiment of the p-nitroiodobenzene in the water body is carried out by sampling and testing an empty solvent, a blank matrix sample and a standard working solution with the lowest grade concentration, wherein the specificity experiment of the p-nitroiodobenzene in the soil is carried out by measuring 0.01mol/L calcium chloride solution blank sample and 0.01mol/L calcium chloride solution adding recovery rate sample by using an established liquid chromatography analysis method, and adding the recovery rate sample, namely, red loam, black soil, brown soil, tide soil, paddy soil blank water sample and soil sample, red loam, black soil, brown soil, tide soil, paddy soil adding recovery rate water sample and soil sample, and comparing spectrograms of the blank sample and the added recovery rate sample; Step four, recovery rate and repeatability experiments, namely, carrying out recovery rate and repeatability experiments on test water, an algae culture medium and an M4 culture medium respectively by setting 1 matrix blank group and 3-grade additive concentration, wherein each grade concentration is 5-grade, the precision of an analysis method is represented by repeatability, the repeatability is represented by Relative Standard Deviation (RSD), the recovery rate is carried out by adopting a recovery rate test solution to analyze, and the RSD of each 5 levels of low, medium and high concentrations is calculated, the recovery rate and the repeatability in soil are as follows, the recovery rate and the repeatability experiments are carried out by setting 5 matrix blank groups and 2-grade additive concentration in soil respectively, 5 samples are prepared in parallel for each grade concentration, the accuracy of the analysis method is represented by average recovery rate, the precision of the analysis method is represented by repeatability, and the Relative Standard Deviation (RSD). Fifthly, setting the detection Limit (LOD) of the method to be 3 times of the baseline noise, namely the concentration corresponding to the target object to be detected when the signal-to-noise ratio is 3, and setting the quantification Limit (LOQ) of the method to be 10 times of the baseline noise, namely the concentration corresponding to the target object to be detected when the signal-to-noise ratio is 10 And step six, analyzing experimental results, wherein the experimental results comprise specificity, linear range and correlation, recovery rate and repeatability, and detection limit and quantitative limit.
2. The method for detecting p-nitroiodobenzene in water and soil based on ultra performance liquid chromatography as claimed in claim 1, wherein in said step one, The instrument for testing the p-nitroiodobenzene in the water body comprises an instrument Agilent 1290-6495A, a detector VWD detector, a sample injection amount of 20.00 mu L, a column temperature of 30.0 ℃, a mobile phase and a ratio (V/V) of acetonitrile to 0.1% phosphoric acid water (70:30), a detection wavelength of 296nm, a running time of 8.00min and a retention time of about 2.9min, wherein the flow rate of the detector is 0.500mL/min; The conditions of the instrument for testing p-nitroiodobenzene in soil are Agilent 1290-6495A, accurasil mm×4.6mm (id), 5 μm (SN: 074263A), VWD as detector, 296nm as detection wavelength, acetonitrile as mobile phase A, 0.1% phosphoric acid water as mobile phase B, 1.000mL/min flow rate, 50.00 μl sample injection amount, 30.0 ℃ column temperature, 15.00min running time, and about 6.1min retention time.
3. The method for detecting p-nitroiodobenzene in water and soil based on ultra performance liquid chromatography as claimed in claim 1, wherein in said step two, Standard stock solution in water is prepared by weighing standard substance p-nitroiodobenzene (0.02006 g), purity of 99.7%, diluting solvent methanol (20.00 mL), constant volume of stock solution concentration of 1000mg/L, and mixing with solvent to scale, and sealing in a refrigerator at 2-8deg.C under dark condition; The preparation of standard stock solution in soil comprises weighing the sample, dissolving with methanol to obtain sample stock solution (STDSTD-1000 ppm), dissolving with calcium chloride solution to obtain sample stock solution (STD-CaCl 2-4.00 ppm) for preparing standard working solution, diluting with acetonitrile for adding recovery rate test; preparing standard working solutions in water, namely taking mother solutions with different concentrations and different removal amounts, and diluting the mother solutions with acetonitrile to obtain the standard working solutions with different concentrations; The preparation of the standard working solution in the soil comprises the steps of taking mother solutions with different concentrations and different removal amounts, and diluting the mother solutions with methanol to obtain the standard working solution with different concentrations.
4. The method for detecting p-nitroiodobenzene in water and soil based on ultra performance liquid chromatography as claimed in claim 1, wherein in said step two, Respectively diluting p-nitroiodobenzene in a water body to obtain a series of standard working solutions, setting 6 calibration points on a standard curve, wherein the linear range is 10.0-500 mug/L, taking the concentration of the p-nitroiodobenzene as an abscissa and the average value of peak areas as an ordinate, and fitting the standard curve by adopting a linear regression equation; And (3) obtaining a series of standard working solutions according to the linearity and the range of the p-nitroiodobenzene in the soil, setting 6 calibration points on a standard curve, acquiring 2 needles for each concentration, taking the concentration of a tested object as an abscissa and the average value of peak areas as an ordinate, and fitting the standard curve by adopting a linear regression equation.
5. The method for detecting p-nitroiodobenzene in water and soil based on ultra performance liquid chromatography as claimed in claim 1, wherein in the fourth step, the recovery rate calculation formula is: Wherein R is the recovery rate, C d is the actual measured concentration of the target object, and C a is the actual addition concentration of the target object; The standard deviation calculation formula is: Wherein S is the standard deviation, x i is the recovery rate obtained by the ith measurement, N is the average value of the recovery rate, and N is the number of the recovery rates participating in calculation; The relative standard deviation calculation formula is: wherein RSD is the relative standard deviation.
6. The method for detecting p-nitroiodobenzene in water and soil based on ultra performance liquid chromatography as claimed in claim 1, wherein in the fifth step, the detection limit of the method has a calculation formula: Wherein LOD is a detection limit, C is the actual added concentration of a low concentration file, R S/N is the signal-to-noise ratio corresponding to the concentration; The quantitative limit calculation formula of the method is as follows: Wherein LOQ is a quantitative limit, C is a theoretical concentration of the low concentration grade addition recovery rate, and R S/N is a concentration corresponding signal to noise ratio.

Description

Method for detecting p-nitroiodobenzene in water body and soil based on ultra-high performance liquid chromatography Technical Field The invention relates to the technical field of water body soil detection, in particular to a method for detecting p-nitroiodobenzene in water body and soil based on ultra-high performance liquid chromatography. Background P-nitroiodobenzene is an important industrial raw material and is widely applied to the fields of chemical synthesis of dyes, pesticides, pharmacy, rubber and the like. However, p-nitroiodobenzene has severe toxicity and potential carcinogenicity, can enter human body through respiratory tract, skin and digestive tract, and cause methemoglobin, and can cause central nervous system injury and hemolytic anemia when severe. In an environment medium, nitrobenzene is difficult to degrade naturally and is easy to accumulate in soil and water, and after being enriched through a food chain, the nitrobenzene forms a long-term threat to the ecosystem and human health. Thus, there is a need for a method for detecting p-nitroiodobenzene in water and soil. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. Disclosure of Invention The invention aims to overcome the technical defects, and provides the method for detecting the p-nitroiodobenzene in the water body and the soil based on the ultra-high performance liquid chromatography, wherein the retention time of the p-nitroiodobenzene in the water body is about 2.9min, the target peak and other components can realize baseline separation under the detection wavelength of 296nm, other impurity interference phenomena are not generated, the method has good selectivity, the retention time of the p-nitroiodobenzene in the soil under the detection wavelength of 296nm is about 6.1min, the target peak can realize baseline separation, the separation degree with other impurity peaks is more than 1.5, and the method has good selectivity. In order to solve the problems, the technical scheme of the invention is a method for detecting p-nitroiodobenzene in water and soil based on ultra-high performance liquid chromatography, which comprises the following steps: Detecting by using an ultra-high performance liquid chromatograph, and determining different detection conditions according to water and soil; step two, preparing a working solution of the detected object, wherein the configuration comprises the configuration of a standard stock solution and the configuration of the standard working solution; The specificity experiment of the p-nitroiodobenzene in the water body is carried out by sampling and testing an empty solvent, a blank matrix sample and a standard working solution with the lowest grade concentration, wherein the specificity experiment of the p-nitroiodobenzene in the soil is carried out by measuring 0.01mol/L calcium chloride solution blank sample and 0.01mol/L calcium chloride solution adding recovery rate sample by using an established liquid chromatography analysis method, and adding the recovery rate sample, namely, red loam, black soil, brown soil, tide soil, paddy soil blank water sample and soil sample, red loam, black soil, brown soil, tide soil, paddy soil adding recovery rate water sample and soil sample, and comparing spectrograms of the blank sample and the added recovery rate sample; Step four, recovery rate and repeatability experiments, namely, carrying out recovery rate and repeatability experiments on test water, an algae culture medium and an M4 culture medium respectively by setting 1 matrix blank group and 3-grade additive concentration, wherein each grade concentration is 5-grade, the precision of an analysis method is represented by repeatability, the repeatability is represented by Relative Standard Deviation (RSD), the recovery rate is carried out by adopting a recovery rate test solution to analyze, and the RSD of each 5 levels of low, medium and high concentrations is calculated, the recovery rate and the repeatability in soil are as follows, the recovery rate and the repeatability experiments are carried out by setting 5 matrix blank groups and 2-grade additive concentration in soil respectively, 5 samples are prepared in parallel for each grade concentration, the accuracy of the analysis method is represented by average recovery rate, the precision of the analysis method is represented by repeatability, and the Relative Standard Deviation (RSD). Fifthly, setting the detection Limit (LOD) of the method to be 3 times of the baseline noise, namely the concentration corresponding to the target object to be detected when the signal-to-noise ratio is 3, and setting the quantification Limit (LOQ) of the method to be 10 times of the baseline noise, name