CN115219627A - Method for detecting acetaldehyde content in leather - Google Patents
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- CN115219627A CN115219627A CN202210842564.4A CN202210842564A CN115219627A CN 115219627 A CN115219627 A CN 115219627A CN 202210842564 A CN202210842564 A CN 202210842564A CN 115219627 A CN115219627 A CN 115219627A
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Abstract
The invention discloses a method for detecting the content of acetaldehyde in leather, which belongs to the technical field of physical and chemical detection and comprises the following steps: adding a phosphoric acid solution into a leather sample for ultrasonic extraction, collecting extract liquor, adding a 2,4-dinitrophenylhydrazine solution into the extract liquor for derivatization, then cooling and filtering, collecting filtrate, and determining the content of acetaldehyde-DNPH derivatives in the filtrate by using a liquid chromatography-tandem mass spectrometry method. The method disclosed by the invention is simple to operate, accurate in qualitative determination, good in sensitivity and precision, and capable of improving the monitoring level of the acetaldehyde content in the leather.
Description
Technical Field
The invention relates to the field of physical and chemical detection, in particular to a method for detecting acetaldehyde content in leather.
Background
Acetaldehyde is a slightly toxic polar organic substance, colorless, flammable, having an irritating odor and being volatile. High concentrations of acetaldehyde can cause acute toxicity, death from pulmonary edema, subacute and chronic toxicity causing central nervous system toxicity, acetaldehyde is also teratogenic, and continued exposure to acetaldehyde can cause serious long-term health risks including cirrhosis of the liver, gastric cancer, esophageal cancer, blood cancer, osteoporosis, and alzheimer's disease, among others. Acetaldehyde in leather is mainly derived from chemicals such as mildew preventive, organic synthetic tanning agent, fixing agent, finishing agent and the like.
In the prior art, the method for detecting the acetaldehyde content is mainly applied to the field of food, and relates to the determination of the acetaldehyde content in leather. Therefore, how to provide a method for accurately detecting the acetaldehyde content in leather is a technical problem which needs to be solved in the field.
Disclosure of Invention
The invention aims to provide a method for detecting acetaldehyde in leather by liquid chromatography-tandem mass spectrometry, which solves the problems in the prior art and can accurately detect the acetaldehyde content in the leather.
In order to achieve the purpose, the invention provides the following scheme:
a method for detecting the acetaldehyde content in leather comprises the following steps:
adding a phosphoric acid solution into a leather sample for ultrasonic extraction, collecting extract liquor, adding a 2,4-dinitrophenylhydrazine solution into the extract liquor for derivatization, then cooling and filtering, collecting filtrate, and determining the content of acetaldehyde-DNPH derivatives in the filtrate by using a liquid chromatography tandem mass spectrometry.
Has the advantages that: the invention applies the detection technology of the liquid chromatogram tandem mass spectrometry, has accurate qualitative and good sensitivity and precision.
Preferably, the leather comprises sheep leather or cow leather.
Has the advantages that: the sheep leather or the cow leather is the most common material in the leather industry at present, and the application field is the widest. The invention utilizes the leather sample to be cut into small pieces with the size not more than 3mm multiplied by 3mm when the sample is prepared, which is beneficial to fully wetting the sample by the extract liquid and ensuring that the acetaldehyde in the sample can be fully extracted.
Preferably, the extraction specifically comprises the following steps:
adding phosphoric acid solution into leather sample, performing ultrasonic extraction at 50 deg.C under 300W for 30min, and vacuum filtering with glass fiber filter to obtain extractive solution.
Has the advantages that: the method adopts different ultrasonic temperatures (20 ℃, 30 ℃, 40 ℃, 50 ℃ and 60 ℃) and ultrasonic times (10 min, 20min, 30min, 40min, 50min, 60min and 70 min) to carry out tests, and the result of the extraction efficiency of the labeled sample with ultrasonic waves at 50 ℃ for 30min is the best.
Preferably, the mass concentration of the phosphoric acid solution is 2.0%;
the ratio of the addition amount of the leather sample to the addition amount of the phosphoric acid solution is 1.0g:10ml.
Has the advantages that: 10ml of phosphoric acid solution allowed complete impregnation of 1.0g of the leather sample.
Preferably, the derivatization treatment specifically comprises the following steps:
adding 1.0mL of 2, 4-dinitrophenylhydrazine solution into 4.0mL of the extraction liquid, diluting the solution to 10mL by using first-order water, fully shaking the solution uniformly, placing the solution in a water bath at 40 ℃ for derivatization treatment for 30min, cooling the solution to room temperature, filtering the solution by using a 0.22-micron polyamide filter membrane, and collecting filtrate.
Preferably, the concentration of the 2,4-dinitrophenylhydrazine solution is 1.0g/L.
Has the advantages that: the invention adopts 2,4-dinitrophenylhydrazine solution with the concentration of 1.0g/L, so that the derivatization is more complete, and the treatment efficiency is highest under the derivatization treatment condition.
Preferably, the liquid chromatography tandem mass spectrometry determination comprises preparation of a standard working solution, liquid chromatography tandem mass spectrometry determination and result calculation.
The liquid chromatography tandem mass spectrometer used in the present invention is AB Qtrap4500.
Preferably, the preparation of the standard working solution comprises the following steps:
0.1mL of acetaldehyde solution with the mass concentration of 1000mg/L is diluted to 100mL by 90% water/10% acetonitrile (namely, solution prepared by 90% water and 10% acetonitrile by volume), so as to obtain 1.0mg/L acetaldehyde standard solution, and then the acetaldehyde standard solution is respectively diluted by 90% water/10% acetonitrile, so as to obtain standard working solution with concentration gradient.
Preferably, the concentration gradient is 0.2. Mu.g/L, 1.0. Mu.g/L, 5.0. Mu.g/L, 10.0. Mu.g/L, 20.0. Mu.g/L.
Preferably, the liquid chromatography tandem mass spectrometer assay comprises the steps of:
sucking prepared standard working solutions with different concentrations, and injecting the standard working solutions into a liquid chromatography tandem mass spectrometer;
wherein the chromatographic column is CQUITY with specification of 100mm × 2.1mm,1.7 μm
A BEH C18 chromatography column;
the mobile phase is a mixed solution of ammonium acetate water solution and acetonitrile, and the flow rate is 0.3mL/min;
the volume ratio of the ammonium acetate aqueous solution to the acetonitrile is 1:4; the concentration of the ammonium acetate aqueous solution is 1mmol/L;
isocratic elution for 0-3 min;
column temperature: 40 ℃; sample introduction amount: 5 mu L of the solution;
the mass spectrometry conditions used were: detecting in an electrospray ion source negative ion scanning mode and a multi-reaction monitoring mode; the voltage of ion spraying is-4500V; the ion source temperature is 450 ℃; atomizing gas pressure is 50.0Psi; air curtain air 50psi; auxiliary heating gas 50.0Psi; collision cell exit voltage-14 eV; the parent ion Q1 is 222.9m/z; the cluster removing voltage is-40V; daughter ion Q3 was 46.2m/z or 121.9am/z; the collision energy is-28V or-48V.
Has the advantages that: in the invention, the mixed solution of ammonium acetate aqueous solution and acetonitrile is selected as the mobile phase, so that the sensitivity of the mobile phase is improved. The BEH C18 column (100 mm. Times.2.1 mm,1.7 μm) has better stability to acidic mobile phases. The acetaldehyde-DNPH derivative is detected in an electric spray ion source negative ion scanning mode and a multi-reaction monitoring mode, and the obtained response value is high.
Preferably, the results are calculated as a quantitative analysis using an external standard method.
Specifically, regression analysis is carried out on the corresponding concentration of the quantitative ion pair peak area of the target object to obtain a standard curve, the correlation coefficient is greater than or equal to 0.999, the extracted sample is measured, the quantitative ion pair peak area ratio of the detected analyte is measured, and the ratio is substituted into the standard curve to obtain the content of acetaldehyde in the sample.
The acetaldehyde-DNPH derivative has good stability, and the standard curve prepared by the method has good linearity, so that the acetaldehyde-DNPH derivative can be quantified by an external standard method.
The invention discloses a method for detecting the content of ethanol in leather, which comprises the steps of carrying out derivatization treatment by using a phosphoric acid solution as an extracting agent and 2,4-dinitrophenylhydrazine as a derivatization reagent, and finally carrying out acetaldehyde content detection by using a liquid chromatography tandem mass spectrometer. The method disclosed by the invention is simple to operate, accurate in qualitative determination, good in sensitivity and precision, and capable of improving the monitoring level of the acetaldehyde content in the leather. Experimental results show that in the detection process, acetaldehyde has good linearity in the range of 0.2-20.0 mug/L, linear correlation coefficients are all larger than 0.999, the standard recovery rate is 83.1-95.2%, precision (RSDs) is less than 5.0%, the detection Limit (LOD) is 2.0 mug/kg, and the quantification Limit (LOQ) is 6.0 mug/kg.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic diagram of the reaction of acetaldehyde with DNPH in example 1 of the present invention;
FIG. 2 is a schematic representation of the reaction of acetaldehyde with MBTH in comparative example 1 of the present invention;
FIG. 3 is a graph showing the effect of different derivatizing reagents on assay recovery in comparative example 1 of the present invention;
FIG. 4 is a graph of acetaldehyde recovery as a function of extraction time for different extraction temperatures in example 2 of the present invention;
FIG. 5 is a graph of acetaldehyde recovery as a function of time from derivatization at different temperatures for example 3 in accordance with the invention;
FIG. 6 is a MS/MS diagram of an acetaldehyde-DNPH derivative in example 5 of the present invention;
FIG. 7 is a MRM chart of an acetaldehyde-DNPH derivative in example 5 of the present invention;
FIG. 8 is a graph of a standard linear regression in example 6 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
A method for detecting the content of acetaldehyde in leather comprises the following steps:
cutting leather into small pieces with the size not more than 3mm multiplied by 3mm as leather samples, uniformly mixing, accurately weighing 1.0g, placing the weighed pieces into a 50mL colorimetric tube with a plug, adding 10mL of 2.0% phosphoric acid solution, and carrying out ultrasonic extraction at the ultrasonic power of 300W for 30min at the temperature of 50 ℃. After extraction, vacuum filtering with glass fiber filter, transferring 4.0mL of the filtered extractive solution into 10mL colorimetric tube with plug, adding 1.0mL of 2,4-Dinitrophenylhydrazine (DNPH) solution with concentration of 1.0g/L, diluting to scale with primary water, shaking thoroughly, and placing in 40 deg.C water bath for derivatization treatment for 30min. After cooling, the mixture was filtered through a 0.22 μm polyamide filter and the filtrate was measured by a liquid chromatography tandem mass spectrometer.
FIG. 1 shows the derivatization reaction of DNPH on leather extract;
the chromatographic mass spectrometry conditions were as follows:
a chromatographic column: ACQUITY
BEH C18 column (100 mm. Times.2.1mm, 1.7 μm); mobile phase: 1mmol/L ammonium acetate water solution and acetonitrile, wherein the volume fraction of the ammonium acetate water solution is 20 percent, and the volume fraction of the acetonitrile is 80 percent; flow rate: 0.3mL/min; isocratic elution procedure: and (3) performing isocratic elution for 0-3 min. Sample introduction amount: 5.0 mu L; column temperature: at 40 ℃.
Electrospray ion source (ESI) negative ion scan mode, multiple reaction monitoring mode detection (MRM); ion spray voltage (IS) -4500V; ion source Temperature (TEM) 450 ℃; atomizing GAS pressure (GAS 1) 50.0Psi; air curtain air (CUR) (50 psi); auxiliary heating GAS (GAS 2) 50.0Psi; collision cell outlet voltage (CXP) -14eV; Q1/Q3 ion pair, declustering voltage (DP) -40V, and Collision Energy (CE) -28V/-48V. The parent ion Q1 was 222.9, the quantitative ion was 166.9, and the qualitative ion was 179.0.
Example 2
Optimization of extraction conditions
A method for detecting acetaldehyde content in leather is different from that in example 1 only in that tests are carried out at different ultrasonic temperatures (20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃) and ultrasonic times (10 min, 20min, 30min, 40min, 50min, 60min, 70 min), and the result of the extraction efficiency of the obtained labeled sample is shown in figure 4. It can be seen that the extraction efficiency is the highest when the ultrasonic temperature is 50 ℃ and the ultrasonic time is 30min.
Example 3
Optimization of derivatization conditions
A method for detecting the content of acetaldehyde in leather is different from that in example 1 only in that experiments are carried out at different derivatization temperatures (20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃) and derivatization times (10 min, 20min, 30min, 40min, 50min, 60min, 70min and 80 min), and the derivatization efficiency results of the obtained labeled samples are shown in figure 5. It can be seen that the derivatization efficiency is best at 40 ℃ and 30min.
Example 4
Selection of mobile phase
The method for detecting the content of acetaldehyde in leather is different from the method in example 1 only in that the influence of three flow-to-DNPH-acetaldehyde derivative chromatographic sensitivities and peak-off times of 1mmol/L ammonium acetate aqueous solution and acetonitrile are respectively 1:1, 2:3 and 1:4. Table 1 shows the influence of the volume ratio of 1mmol/L ammonium acetate aqueous solution to acetonitrile on the peak-off time and the response value, and the combination of Table 1 shows that the three mobile phases achieve the detection purpose on DNPH-acetaldehyde derivatives, but the sensitivity is relatively good when the volume ratio of 1mmol/L ammonium acetate aqueous solution to acetonitrile is 1:4 (namely the volume fractions are 20% and 80% respectively) as the mobile phases, the peak-off time is early, the detection speed can be effectively improved, and the reagent cost is saved.
Table 1:
| volume ratio of | Time to peak/min | Response value |
| 1:1 | 3.42 | 406482 |
| 2:3 | 2.34 | 440325 |
| 1:4 | 1.62 | 462510 |
Example 5
Selection of Mass Spectrometry conditions
After the derivatization reaction between 10.0. Mu.g/L acetaldehyde solution and 1.0 g/L2,4-dinitrophenylhydrazine solution is completed, the reaction solution is injected into an ESI source, and continuous injection is carried out by a peristaltic pump, and scanning analysis is respectively carried out by ESI (+) and ESI (-) ion modes. The MS/MS mass spectrum of the acetaldehyde-DNPH derivative after the optimization of mass spectrum conditions is shown in FIG. 6, and the MRM diagram is shown in FIG. 7. As can be seen from FIGS. 6 and 7, the retention time of the quantitative ion pair 222.9 → 46.2 and the retention time of the qualitative ion pair 222.9 → 121.9 are 1.62min. Experimental results show that the intensity of the protonated molecular ion peak obtained by scanning in the ESI (-) ion mode is high, and the stability is good.
Example 6
Method detection limit and linear relation
0.2 mug/L, 1.0 mug/L, 5.0 mug/L, 10.0 mug/L and 20.0 mug/L series standard solutions are prepared in the concentration range of 0.2 mug/L-20.0 mug/L. The prepared standard solution was derivatized with DNPH solution and then tested with a liquid chromatography tandem mass spectrometer (derivatization, i.e., chromatographic mass spectrometry conditions were the same as in example 1). The data obtained were linearly regressed (as shown in FIG. 8) for peak area (y) with acetaldehyde content (x, μ g/L) to obtain a linear regression equation and correlation coefficients for the standard curve. The mass concentration corresponding to the signal-to-noise ratio (S/N = 3) was calculated by weighing 1.0g, and was defined as the limit of detection (LOD). The linear range of acetaldehyde mass concentration, the linear regression equation, the correlation coefficient and the detection limit are shown in table 2.
TABLE 2 Linear range of acetaldehyde mass concentration, linear regression equation, correlation coefficient and detection limit
Example 7
Method recovery and precision
Two negative samples of cow leather and sheep leather were selected, and 1.0. Mu.g/L, 5.0. Mu.g/L, and 20.0. Mu.g/L acetaldehyde standard solutions were added, respectively, and the prepared standard solutions were subjected to derivatization with DNPH solution, and then tested with a liquid chromatography tandem mass spectrometer (the conditions of derivatization, i.e., chromatographic mass spectrometry, were the same as in example 1). The average recovery and precision [ in terms of Relative Standard Deviations (RSDs) ] were calculated for 6 replicates per spiked level and the results are shown in table 3.
Table 3 mean recovery and Relative Standard Deviation (RSD) measurements (n = 6)
As can be seen from Table 3, the recovery rate of the acetaldehyde content test is 83.1-95.2%, and the precision is 2.7-3.9%.
Comparative example 1
A method for detecting acetaldehyde content in leather, which is different from that in example 1 only in that a phenol reagent (MBTH) is used as a derivatization reagent to perform derivatization treatment on an extraction liquid, and a schematic diagram of the derivatization reaction of the MBTH on the leather extraction liquid is shown in fig. 2. The effect of the results of the measurements on leather samples of example 1 and comparative example 1 by different addition amounts (1.0. Mu.g/L, 5.0. Mu.g/L, 20.0. Mu.g/L concentration of acetaldehyde standard solution) is shown in FIG. 3.
As can be seen from FIG. 3, the DNPH derivatization effect is better than that of MBTH.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. The method for detecting the acetaldehyde content in leather is characterized by comprising the following steps:
adding a phosphoric acid solution into a leather sample for ultrasonic extraction, collecting extract liquor, adding a 2,4-dinitrophenylhydrazine solution into the extract liquor for derivatization, then cooling and filtering, collecting filtrate, and determining the acetaldehyde content in the filtrate by using a liquid chromatography-tandem mass spectrometry method.
2. The method for detecting acetaldehyde content in leather according to claim 1, wherein the leather comprises sheep leather or cow leather.
3. The method for detecting the acetaldehyde content in leather according to claim 1, wherein the extraction specifically comprises the following steps:
adding phosphoric acid solution into leather sample, performing ultrasonic extraction at 50 deg.C under 300W for 30min, and vacuum filtering with glass fiber filter to obtain extractive solution.
4. The method for detecting the acetaldehyde content in the leather according to claim 3, wherein the phosphoric acid solution is 2.0% by mass;
the ratio of the addition amount of the leather sample to the addition amount of the phosphoric acid solution is 1.0g:10ml.
5. The method for detecting the acetaldehyde content in leather according to claim 1, wherein the derivatization treatment specifically comprises the following steps:
adding 1.0mL of 2, 4-dinitrophenylhydrazine solution into 4.0mL of the extraction liquid, diluting to 10mL by using first-order water, fully shaking up, placing in a water bath at 40 ℃ for derivatization treatment for 30min, then cooling to room temperature, filtering by using a 0.22-micron polyamide filter membrane, and collecting filtrate.
6. The method for detecting the acetaldehyde content in the leather according to claim 5, wherein the concentration of the 2,4-dinitrophenylhydrazine solution is 1.0g/L.
7. The method for detecting the acetaldehyde content in the leather according to claim 1, wherein the liquid chromatography tandem mass spectrometry measurement comprises preparation of a standard working solution, measurement of a liquid chromatography tandem mass spectrometer and result calculation.
8. The method for detecting the acetaldehyde content in the leather according to claim 7, wherein the preparation of the standard working solution comprises the following steps:
0.1mL of acetaldehyde solution with the mass concentration of 1000mg/L is diluted to 100mL by 90% water/10% acetonitrile to obtain 1.0mg/L acetaldehyde standard solution, and then the acetaldehyde standard solution is respectively diluted by 90% water/10% acetonitrile to obtain standard working solution with concentration gradient.
9. The method for detecting the acetaldehyde content in the leather according to claim 7, wherein the liquid chromatography tandem mass spectrometry comprises the following steps:
sucking prepared standard working solutions with different concentrations, and injecting the standard working solutions into a liquid chromatography tandem mass spectrometer;
wherein the chromatographic column has specification of 100mm × 2.1mm,1.7 μm
A BEH C18 chromatography column;
the mobile phase is a mixed solution of ammonium acetate water solution and acetonitrile, and the flow rate is 0.3mL/min;
the volume ratio of the ammonium acetate aqueous solution to the acetonitrile is 1:4; the concentration of the ammonium acetate aqueous solution is 1mmol/L;
isocratic elution for 0-3 min;
column temperature: 40 ℃; sample introduction amount: 5 mu L of the solution;
the mass spectrometry conditions used were: detecting in an electrospray ion source negative ion scanning mode and a multi-reaction monitoring mode; the voltage of ion spraying is-4500V; the ion source temperature is 450 ℃; the atomizing gas pressure is 50.0Psi; air curtain air 50psi; auxiliary heating gas 50.0Psi; collision cell exit voltage-14 eV; the parent ion Q1 is 222.9m/z; the cluster removing voltage is-40V; daughter ion Q3 was 46.2m/z or 121.9am/z; the collision energy is-28V or-48V.
10. The method for detecting the acetaldehyde content in leather according to claim 7, wherein the result is calculated by quantitative analysis using an external standard method.
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