CN113960188A - High performance liquid chromatography-tandem mass spectrometry method for determining 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in sample - Google Patents
High performance liquid chromatography-tandem mass spectrometry method for determining 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in sample Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 41
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- 238000010828 elution Methods 0.000 claims description 23
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 14
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- 238000002552 multiple reaction monitoring Methods 0.000 claims description 5
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 4
- 238000002137 ultrasound extraction Methods 0.000 claims description 4
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Abstract
The invention relates to the technical field of compound analysis and detection, in particular to a method for determining 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in a sample by using a high performance liquid chromatography-tandem mass spectrometry method. The method comprises the following steps: the pretreatment adopts an extraction solvent-ultrasonic combined mode to extract a sample; and simultaneously optimizing the chromatographic conditions of the high performance liquid chromatography-tandem mass spectrometry. The invention firstly proposes to detect the residue of 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in a sample by adopting high performance liquid chromatography-tandem mass spectrometry through analyzing the physical properties of the substance; and by optimizing the detection conditions, the peak shape with good symmetry, narrow peak width and high response and without impurity peak interference near the retention time is finally obtained, and the peak emergence time of the target compound is earlier than the impurity peak and is completely separated from the impurity peak, so that the detection accuracy is greatly improved.
Description
Technical Field
The invention relates to the technical field of compound analysis and detection, in particular to a method for determining 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in a sample by using a high performance liquid chromatography-tandem mass spectrometry method.
Background
4, 4-bis (dimethylamino) -4-methylaminotrityl Alcohol is a dye compound, has the name of 4,4 '-bis (dimethylamino) -4' - (dimethylamino) Trityl Alcohol and the molecular formula of C24H29N3O, CAS NO: 561-41-1, structural formula as follows:
the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol has the advantages of good performance, economy, wide adaptability and the like, and is widely applied to the field of coloring products such as textiles, printing ink and the like. However, it has been found that it is highly irritating to the eye and carcinogenic to prolonged exposure, and it is therefore necessary to detect residual 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol in the product.
Through retrieval, the detection technology of 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol is rarely reported at present, but the existing detection method of the printing and dyeing compound residue is not suitable for the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol, has the problems of inaccurate detection result or complex detection process, and is difficult to provide convenient and effective technical support for the safe export of products.
Disclosure of Invention
Aiming at the technical problems, the invention develops a quantitative detection method aiming at the content of 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in a sample by exploring and optimizing the analysis conditions of an instrument according to the physicochemical properties and characteristics of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol, and provides simple, convenient and accurate technical support for the export detection of the substance.
The method for analyzing and detecting the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol comprises the following steps: pretreating a sample, and analyzing and detecting the treated sample by adopting a high performance liquid chromatography-tandem mass spectrometry; wherein:
the pretreatment adopts an extraction solvent-ultrasonic combined mode to extract a sample;
the operating conditions of the high performance liquid chromatography-tandem mass spectrometry are as follows:
mobile phase: formic acid water-acetonitrile;
the elution procedure is table 1;
TABLE 1
| Time (min) | A(％) | B(％) |
| 0.00 | 50～100 | 0～50 |
| 1.00 | 0～50 | 50～100 |
| 2.50 | 0～50 | 50～100 |
| 3.00 | 50～100 | 0～50 |
| 3.50 | 50～100 | 0～50 |
The invention establishes a set of rapid detection method aiming at the substance for the first time through the physical analysis of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol and the common products containing the substance residue.
The invention provides a method for detecting the residual quantity of a substance in a sample by adopting a combined mode of ultrasonic extraction and high performance liquid chromatography-tandem mass spectrometry. On one hand, the invention adopts the combined mode of extraction solvent-ultrasound to extract the sample, thereby avoiding the introduction of impurities due to over-extraction and influencing the accuracy of the detection result while ensuring the extraction rate. On the other hand, the invention adopts the high performance liquid chromatography-tandem mass spectrometry to detect the target compound, optimizes the mobile phase and the elution program, avoids the elution phase from forming bubbles in a chromatographic column or a detector and influencing the separation, improves the separation degree, and finally obtains the peak shape which has good symmetry, narrow peak width and high response and has no impurity peak interference near the retention time; and the control condition is adopted, so that the peak emergence time of the target compound is earlier than the impurity peak, and the target compound is completely separated from the impurity peak, and the detection accuracy is greatly improved.
The applicant intends to emphasize here that although hplc-tandem mass spectrometry is a common technical means in the field, based on the physical properties of the target compound and the sample, the selection of different pre-treatments and detection methods and the optimization of conditions have a great influence on the accuracy and detection efficiency of the detection result, and are difficult to predict by those skilled in the art, and therefore, the detection result needs to be obtained by research and development personnel through a large number of experiments. Therefore, the method for detecting the residual 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol in the sample is not obvious.
Preferably, the pH of the formic acid solution in the formic acid solution-acetonitrile is 3 to 6, and more preferably 3.
Preferably, the elution procedure is as in table 2.
TABLE 2
| Time (min) | A(％) | B(％) |
| 0.00 | 80 | 20 |
| 1.00 | 20 | 80 |
| 2.50 | 20 | 80 |
| 3.00 | 80 | 20 |
| 3.50 | 80 | 20 |
As one embodiment of the present invention, the chromatographic conditions are:
a chromatographic column: agilent Zorbax Eclipse XDB-C18(2.1 x 100mm,3.5 μm);
sample introduction amount: 2-10 mu L;
column temperature: 40 ℃;
mobile phase: aqueous formic acid (pH ═ 3) (a) and acetonitrile (B);
flow rate: 0.1-0.4 mL/min;
and (3) an elution mode: gradient elution was used and the elution procedure is detailed in table 2.
Research results show that under the condition, the response value of the instrument is obviously improved, the peak shape is sharp, the symmetry is good, no impurity peak interference exists near the retention time, and the sensitivity and the accuracy of detection are further improved.
Further, methanol is selected as the extraction solvent in the present invention. Compared with other extracting agents, the extracting agent has better matching degree with a sample and a target compound, and can further improve the extraction rate and the accuracy of a detection result.
Furthermore, the invention also researches the influence of the extraction temperature and the ultrasonic time on the detection result in the pretreatment. According to the research result, the extraction temperature is determined to be 30-60 ℃, and the ultrasonic time is 30-70 min; under the condition, the extraction time can be shortened as much as possible on the premise of ensuring complete extraction, and the extraction efficiency is improved.
As another embodiment of the present invention, the pretreatment is: carrying out ultrasonic extraction on the sample at 55-60 ℃ for 60-70min according to the proportion of 1g of sample to 5-15 mL of extraction solvent; filtration through a 0.22 μm filter.
Furthermore, the invention also optimizes the mass spectrum condition. The mass spectrum conditions of the high performance liquid chromatography-tandem mass spectrometry are as follows:
capillary voltage: 3500V;
temperature of the desolventizing gas: 320 ℃;
flow rate of desolventizing agent: 5L/min;
temperature of sheath gas: at 330 ℃;
the flow rate of the sheath gas: 11L/min;
multiple reaction monitoring mode.
The parent ions, the daughter ions, the fragmentation voltage and the collision energy are shown in Table 3;
TABLE 3
Further, the linear equation of the target compound of the present invention is: Y96.7X +163.4, wherein: x is mass concentration (. mu.g/L) and Y is peak area.
The research result shows that 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol shows good linear relation in the linear range of 10 mu g/L-200 mu g/L, and the correlation coefficient is 0.9999. On the basis, the detection Limit (LOD) and the quantification Limit (LOQ) of the standard substance are determined by 3-fold and 10-fold signal-to-noise ratios (S/N), and the detection limit of the method is 0.35 mu g/L, and the quantification limit is 1.17 mu g/L.
Meanwhile, research results also show that the standard recovery rate of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol is 98.5-100.6%, and the relative standard deviation of the recovery rate is not more than 2.8%, which indicates that the test method has high accuracy and can meet the test requirements.
As one embodiment of the present invention, the method for measuring 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol comprises the steps of:
(1) pretreatment conditions
Taking methanol as an extraction solvent, and carrying out ultrasonic extraction on a sample at 55-60 ℃ for 60-70min according to the proportion of 1g of sample to 5-15 mL of extraction solvent; filtering with 0.22 μm filter membrane;
(2) the determination of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol was carried out by high performance liquid chromatography-tandem mass spectrometry:
wherein, the chromatographic conditions are as follows:
a chromatographic column: agilent Zorbax Eclipse XDB-C18(2.1 x 100mm,3.5 μm); sample introduction amount: 5 mu L of the solution; column temperature: 40 ℃; mobile phase: aqueous formic acid (pH ═ 3) (a) and acetonitrile (B); flow rate: 0.3 mL/min; and (3) an elution mode: gradient elution was used and the elution procedure is detailed in table 2.
Wherein, the mass spectrum conditions are as follows:
capillary voltage: 3500V; temperature of the desolventizing gas: 320 ℃; flow rate of desolventizing agent: 5L/min; temperature of sheath gas: at 330 ℃; the flow rate of the sheath gas: 11L/min; multiple reaction monitoring mode. The parent ions, the daughter ions, the fragmentation voltage and the collision energy are shown in Table 3.
(3) Calculating the mass concentration of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol according to the obtained peak area;
the calculation formula is as follows: Y96.7X + 163.4;
wherein: x is mass concentration (. mu.g/L) and Y is peak area.
The invention also provides the application of the analysis and detection method in products containing 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol; the product is a textile product, a plastic product or a leather product.
The invention has the following beneficial effects:
the method adopts high performance liquid chromatography-tandem mass spectrometry to detect the residual quantity of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in the printing and dyeing sample according to the characteristics of the residual 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in the printing and dyeing sample, and improves the accuracy, sensitivity and convenience of a detection result by optimizing pretreatment and detection conditions. The determination method provided by the invention has a good linear relation in a linear range of 10-200 mug/L, the detection limit is low, and the relative standard deviation of the recovery rate is not more than 2.8%. The detection method provided by the invention fills the technical blank that the prior art lacks relevant effective detection means, and provides convenient and effective technical support for the safe export of products.
Drawings
FIG. 1 is a total ion chromatogram of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol under optimized conditions.
FIG. 2 is a total ion flux chromatogram of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol at a relatively high initial organic solvent ratio.
FIG. 3 shows the average recovery of different extraction solvents.
FIG. 4 shows the average recovery for different extraction temperatures.
FIG. 5 shows the average recovery for different extraction times.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Each of the components in the following examples is commercially available.
Example 1
The embodiment provides a method for detecting residual 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol in a sample by adopting a high performance liquid chromatography-tandem mass spectrometry method, wherein the sample is a railway vehicle interior seat cover, and the method comprises the following specific steps:
1. early preparation
1.1 Main instruments and reagents
Liquid chromatography: agilent 1290 Infinity II, ms spectrum: 6460 Agilent Triple Quad, all Agilent Inc. USA;
an ultrasonic cleaner: 2300 HT, shanghai' an spectral science instruments ltd;
precision electronic analytical balance: XA205DU, sensory 0.1mg, Metler Switzerland;
a vortex mixer: XW-80A, Shanghai Jingke industries, Ltd;
an ultra-pure water machine: Milli-Q, Millipore, USA;
standard substance: 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol, purity greater than 75%, Toronto Research Chemicals, Canada;
other reagents: methanol, acetonitrile, acetone, dichloromethane, tetrahydrofuran, all HPLC grade, Sigma usa; ammonium acetate, HPLC grade, shanghai mclin biochem ltd.
1.2 preparation of the solution
Standard stock solutions: accurately weighing 10mg of 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol (accurate to 0.1mg) by using a precise electronic analytical balance, dissolving the methyl alcohol and fixing the volume to 10mL to obtain 1000mg/L stock solution, and storing the stock solution in a refrigerator at the temperature of 4 ℃.
Standard working solution: the standard stock solution was diluted stepwise with methanol to obtain 10. mu.g/L, 20. mu.g/L, 50. mu.g/L, 100. mu.g/L, and 200. mu.g/L series of standard working solutions.
1.3 chromatographic conditions
A chromatographic column: agilent Zorbax Eclipse XDB-C18(2.1 x 100mm,3.5 μm); sample introduction amount: 5 mu L of the solution; column temperature: 40 ℃; mobile phase: aqueous formic acid (pH ═ 3) (a) and acetonitrile (B); flow rate: 0.3 mL/min; and (3) an elution mode: gradient elution was used and the elution procedure is detailed in table 2.
1.4 Mass Spectrometry conditions
Under the positive ion mode of an electrospray ion source, firstly, carrying out full scanning on a standard substance solution to obtain stable parent ions, and selecting an ion Scanning (SIM) mode to optimize fragmentation voltage (fragment); and then, carrying out sub-ion scanning, and selecting a characteristic ion pair with a high response value as a quantitative and qualitative ion pair to further optimize Collision Energy (CE). The optimized mass spectrum conditions are as follows:
capillary voltage: 3500V; temperature of the desolventizing gas: 320 ℃; flow rate of desolventizing agent: 5L/min; temperature of sheath gas: at 330 ℃; the flow rate of the sheath gas: 11L/min; multiple reaction monitoring mode. The parent ions, the daughter ions, the fragmentation voltage and the collision energy are shown in Table 3.
1.5 pretreatment conditions
Taking a sample, cutting into pieces with the size not larger than 2mm multiplied by 2 mm. 1g of the minced sample (accurate to 0.1mg) was accurately weighed into a sample vial, and 10mL of methanol was added thereto. And (4) screwing the bottle cap, putting the sample bottle into an ultrasonic cleaning instrument, and performing ultrasonic treatment at 60 ℃ for 60 min. 1mL of the cooled extract was filtered through a 0.22 μm filter and directly measured.
2 results and discussion
2.1 selection of the Mobile phase
Test group 1: using formic acid water-acetonitrile as a mobile phase;
control group 1: selecting methanol as a mobile phase;
control group 2: selecting ammonium acetate as a mobile phase;
the result shows that the peak shape of the test group 1, 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol taking the formic acid water-acetonitrile as the mobile phase is symmetrical, the peak width is narrow, the response is high, and no impurity peak interference exists near the retention time.
The control group 1, 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol with methanol as the mobile phase has low response, trailing peak shape and late peak emergence time;
the control group of 2, 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol using ammonium acetate as the mobile phase had a low response and a broad peak width.
The influence of the pH of the formic acid water on chromatographic peaks was also investigated during the experiment. The result shows that the peak shape of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol is not influenced in the pH range of 3-6.
And finally, selecting formic acid water (pH is 3) -acetonitrile as a mobile phase, and under the optimized chromatographic condition, enabling 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol to peak in 1.80min, and completing the analysis and detection of one sample in 3.5 min.
FIG. 1 is a MRM total ion flux chromatogram of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol. It can be seen from the figure that the peak shape of the substance is sharp, the symmetry degree is good, and the response is also high.
2.2 optimization of elution ratio
Test group 2: aqueous formic acid (pH 3) (a) and acetonitrile (B) were used as mobile phases, and the elution ratios were:
within 0.0-1.0 min, gradually increasing the proportion of acetonitrile from 20% to 80%, and keeping for 1.5 min;
within 2.5-3.0 min, the proportion of acetonitrile is gradually reduced from 80% to 20%, and the acetonitrile is kept for 0.5 min.
Under the elution conditions, 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol showed a peak at 1.80min, impurities showed a peak at 2.55min, and the chromatographic peak of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol was completely separated from the impurity peak, as shown in FIG. 1.
Control group 3: aqueous formic acid (pH 3) (a) and acetonitrile (B) were used as mobile phases, and the elution ratios were:
within 0.0-1.0 min, gradually increasing the proportion of acetonitrile from 50% to 100%, and keeping for 1.5 min;
within 2.5-3.0 min, the proportion of acetonitrile is gradually reduced from 100% to 50%, and the acetonitrile is kept for 0.5 min.
Under the elution condition, 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol peaks at 1.30min, and due to the fact that the proportion of the initial organic solvent is high, the peak time of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol is early, the chromatographic peak contains an impurity peak, and effective separation cannot be achieved, and the detailed chart is shown in fig. 2.
2.3 selection of extraction solvent
Methanol, acetonitrile, acetone, tetrahydrofuran and dichloromethane are selected as extraction solvents, the extraction efficiency of the extraction solvents on 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol in a sample in a high performance liquid chromatography detection method is examined, and the result is shown in figure 3.
The result shows that the average extraction efficiency of methanol, acetonitrile and acetone in the five extraction solvents can reach more than 85 percent under the condition of the same detector. The average extraction efficiency of tetrahydrofuran and dichloromethane to 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol is lower than 80 percent, and the test requirements can not be met. Methanol is preferable as the extraction solvent for the pretreatment in view of the safety and price of the solvent.
2.4 selection of extraction temperature and time
The average recovery was examined at different extraction temperatures and times. As shown in fig. 4 and 5.
As can be seen from fig. 4 and 5, the recovery rate was 85% or more at an ultrasonic temperature of 60 ℃. When the ultrasonic time reaches 60min, the maximum extraction efficiency can be basically reached.
2.5 Linear Range and detection Limit
Under the optimized conditions, the linear range determination and the lowest detection limit test are carried out on the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol.
The standard stock solution is diluted by methanol to 10 mug/L, 20 mug/L, 50 mug/L, 100 mug/L and 200 mug/L series of standard working solutions.
And drawing a standard working curve by taking the mass concentration X (mu g/L) as an abscissa and taking the peak area Y as an ordinate. The linear equation and the correlation coefficient of the obtained substance to be measured are shown in Table 4.
As can be seen from the data in the table, in the linear range of 10 mug/L-200 mug/L, 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol shows good linear relation, and the correlation coefficient is 0.9999.
On the basis, the detection Limit (LOD) and the quantification Limit (LOQ) of the standard substance are determined by 3-fold and 10-fold signal-to-noise ratios (S/N), and the detection limit of the method is 0.35 mu g/L, and the quantification limit is 1.17 mu g/L.
TABLE 4
2.6 recovery and precision
The experiment was carried out by a blank matrix spiking experiment, using samples without 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol as blank matrix, with 3 different spiking concentration levels (10. mu.g/L, 50. mu.g/L, 200. mu.g/L) being set. Each spiked level was tested in parallel 6 times (n-6) for precision.
Under 3 standard adding levels, the standard adding recovery rate of 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol is 98.5-100.6%, and the relative standard deviation of the recovery rate is not more than 2.8%, which indicates that the test method has high accuracy and can meet the test requirements.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. An analytical detection method for 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol, comprising: pretreating a sample, and analyzing and detecting the treated sample by adopting a high performance liquid chromatography-tandem mass spectrometry; wherein:
the pretreatment adopts an extraction solvent-ultrasonic combined mode to extract a sample;
the chromatographic conditions of the high performance liquid chromatography-tandem mass spectrometry are as follows:
mobile phase: formic acid water-acetonitrile;
the elution procedure was:
2. the method for analyzing and detecting 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol according to claim 1, wherein the pH of the aqueous formic acid in the aqueous formic acid-acetonitrile is 3 to 6.
3. The method for the analytical detection of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol according to claim 2, wherein the elution procedure is:
4. the method for the analytical detection of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol according to claim 2, wherein the chromatographic conditions are:
a chromatographic column: agilent Zorbax Eclipse XDB-C18(2.1 x 100mm,3.5 μm);
sample introduction amount: 2-10 mu L;
column temperature: 40 ℃;
mobile phase: aqueous formic acid (pH ═ 3) (a) and acetonitrile (B);
flow rate: 0.1-0.4 mL/min;
and (3) an elution mode: gradient elution was used.
5. The method for the analytical detection of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol as claimed in any of claims 1 to 4, wherein the extraction solvent is methanol.
6. The method for analyzing and detecting 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol as claimed in claim 5, wherein the temperature of the extraction is 30-60 ℃ and the time is 30-70 min.
7. The method for the analytical detection of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol as claimed in any one of claims 1 to 4 and 6, wherein the mass spectrometric conditions of the HPLC-MS are as follows:
capillary voltage: 3500V;
temperature of the desolventizing gas: 320 ℃;
flow rate of desolventizing agent: 5L/min;
temperature of sheath gas: at 330 ℃;
the flow rate of the sheath gas: 11L/min;
multiple reaction monitoring mode.
8. The analytical detection method for 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol according to any one of claims 1 to 4 and 6, further comprising: calculating the mass concentration of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol according to the obtained peak area;
the calculation formula is as follows: Y96.7X + 163.4;
wherein: x is mass concentration, mu g/L;
and Y is a peak area.
9. The method for the analytical detection of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol according to claim 1, comprising the steps of:
(1) sample pretreatment
Taking methanol as an extraction solvent, and carrying out ultrasonic extraction on a sample at 55-60 ℃ for 60-70min according to the proportion of 1g of sample to 5-15 mL of extraction solvent; filtering with 0.22 μm filter membrane;
(2) the determination of 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol was carried out by high performance liquid chromatography-tandem mass spectrometry:
chromatographic conditions are as follows:
a chromatographic column: agilent Zorbax Eclipse XDB-C18;
sample introduction amount: 5 mu L of the solution;
column temperature: 40 ℃;
mobile phase: formic acid in water at pH 3; acetonitrile;
flow rate: 0.3 mL/min;
and (3) an elution mode: gradient elution is adopted;
the mass spectrometry conditions were as follows:
capillary voltage: 3500V; temperature of the desolventizing gas: 320 ℃; flow rate of desolventizing agent: 5L/min; temperature of sheath gas: at 330 ℃; the flow rate of the sheath gas: 11L/min; a multiple reaction monitoring mode;
(3) calculating the mass concentration of the 4, 4-bis (dimethylamino) -4-methylamino trityl alcohol according to the obtained peak area;
the calculation formula is as follows: Y96.7X + 163.4;
wherein: x is mass concentration, mu g/L; and Y is a peak area.
10. Use of an assay according to any one of claims 1 to 9 in a product containing 4, 4-bis (dimethylamino) -4-methylaminotrityl alcohol; the product is a textile product, a plastic product or a leather product.
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