CN108205036B - Method for detecting dibromoneopentyl glycol in textile - Google Patents
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Abstract
The invention discloses a method for detecting dibromoneopentyl glycol in a textile, which comprises the following steps: sample pretreatment: adding acetone into a sample to be detected, carrying out ultrasonic extraction, and taking an extracting solution to obtain a solution to be detected; gas chromatography-mass spectrometry detection: carrying out gas chromatography-mass spectrometry detection on the filtrate, and quantifying by an external standard method, wherein the conditions of the gas chromatography are as follows: a chromatographic column: DB-624 capillary chromatography column; adopting a programmed temperature rise; sample inlet temperature: 230-260 ℃; sample introduction mode: no flow diversion; the mass spectrum conditions are as follows: electron bombardment ionization, ion source temperature: 200-230 ℃; gas chromatography-mass spectrometry interface temperature: 230-280 ℃; an acquisition mode: a full scan mode and a selective ion scan mode. The detection method has the advantages of high detection speed, low detection limit of 0.045mg/L, standard recovery rate of 99.4-100.7% and relative standard deviation of no more than 3.6%.
Description
Technical Field
The invention relates to the field of flame retardant analysis and determination, in particular to a method for detecting dibromoneopentyl glycol in textiles.
Background
Dibromo neopentyl glycol is a reactive flame retardant with excellent performance. The flame-retardant fiber is suitable for unsaturated polyester resin, thermoplastic resin and polyurethane resin, can also be used for rigid polyurethane foam, is added into a polymer, and the prepared polymer has excellent flame retardance, light stability and chemical resistance, is small in dosage and has no influence on the mechanical property of a base resin, particularly, the mixture of the flame-retardant fiber and antimony trioxide is particularly suitable for flame-retardant fibers, the mixture and a high polymer can form a melt with good fluidity and spinnability, and the obtained flame-retardant fibers have good mechanical property. Thus, dibromoneopentyl glycol is widely used in apparel and footwear textiles.
It has been shown that dibromoneopentyl glycol can cause irritation to eyes, skin and respiratory tract, and carcinogenicity may exist. Recently, organizations dedicated to zero emission of hazardous chemicals (ZDHC) have updated the list of limiting substances (MRSL) in manufacturing processes. Dibromo neopentyl bis (2,2-bis (bromomethyl) -1,3-propanediol DBNPG) is included in the list. The list is jointly issued by three environmental organizations in europe with a plurality of clothing known brands, including: adedas, Burberry, C & A, SRRIT, Gap Inc., G-STARRAW, H & M, INDEX, JACKWolfskin, Lbrads, LEVISTA RAUSS & CO, Lining, M & S, New Bailon, Nack, Biao Ma, PVH, UNITED COLORS OF BENETTONL. According to the harmful chemical zero emission program, related brand members of the ZDHC will implement a restricted bill of materials for apparel footwear products.
At present, much research is carried out on the dibromo neopentyl glycol in the synthesis and application fields, and detection on residues of the dibromo neopentyl glycol in products is rarely reported. The method is not only tedious and time-consuming, and poor in accuracy, but also quantifies the product dibromo neopentyl glycol, but also does not qualitatively and quantitatively analyze the content of the dibromo neopentyl glycol in the textile, and the existing technology is difficult to realize qualitative and quantitative analysis of the dibromo neopentyl glycol in the textile.
Disclosure of Invention
Based on the method, the defects of the prior art are overcome, and the method for detecting the dibromoneopentyl glycol in the textile is used for analyzing and testing by adopting a gas chromatography-mass spectrometry combined technology, and has the advantages of high detection speed, high accuracy, good reproducibility, good product separation effect, low detection limit, good standard adding recovery rate and high precision.
The technical scheme is as follows:
a method for detecting dibromoneopentyl glycol in textiles comprises the following steps:
sample pretreatment: adding acetone into a sample to be detected, carrying out ultrasonic extraction, and taking an extracting solution to obtain a solution to be detected;
gas chromatography-mass spectrometry detection: carrying out gas chromatography-mass spectrometry detection and external standard method quantification on the solution to be detected, wherein,
the conditions of the gas chromatography were: a chromatographic column: DB-624 capillary chromatography column; adopting a programmed temperature rise; sample inlet temperature: 230-260 ℃; carrier gas: the flow rate is 1.2-2.0 mL/min; sample introduction mode: no flow diversion;
the mass spectrum conditions are as follows: electron bombardment ionization, ion source temperature: 200-230 ℃; gas chromatography-mass spectrometry interface temperature: 230-280 ℃; solvent delay time: 3-6 min; an acquisition mode: a full scan mode and a selective ion scan mode.
The inventor finds through experiments that when the parameters of the gas chromatography and the mass spectrum are set according to the chromatographic conditions, the dibromoneopentyl glycol in the textile can be accurately qualitatively and quantitatively analyzed by adopting a gas chromatography-mass spectrum combined technology, and the detection method has the advantages of high accuracy of detection results, short detection time, good recovery rate and high precision.
In one embodiment, the gas chromatography conditions are: a chromatographic column: DB-624 capillary chromatography column 30m × 250 μm × 1.40 μm; temperature rising procedure: the initial temperature is 120-160 ℃, the temperature is kept for 0.5-2 min, then the temperature is increased to 230-260 ℃ at the speed of 15-30 ℃/min, the temperature is kept for 5-9 min, and the temperature of a sample inlet is 230-260 ℃; carrier gas: high purity helium with purity > 99.999%; flow rate: 1.2-2.0 mL/min; no shunt sampling; the injection volume is 1-2 mu L.
In one embodiment, the temperature raising procedure: the initial temperature is 150 deg.C, and the temperature is maintained for 1min, and then increased to 250 deg.C at a rate of 25 deg.C/min, and maintained for 6 min.
In one embodiment, the mass spectrometry conditions are electron bombardment ionization, electron energy: 70 eV; ion source temperature: 200-230 ℃; GC-MS interface temperature: 230-280 ℃; temperature of the quadrupole rods: 150 ℃; solvent retardation: 3-6 min; ion scanning quantification was selected with full scan qualitative.
In one embodiment, the full scan qualitatively determines the ions as 214, 133, 151 and the select ion scan quantitatively determines the ions as 214.
In one embodiment, the sample pre-treatment is: taking a sample to be detected, shearing the sample to be detected into a size of 2-5 mm multiplied by 2-5 mm, weighing 0.5-2.0 g, adding 5-20 mL of acetone, carrying out ultrasonic extraction for 45-90 min, filtering an extracting solution by using a microporous filter membrane, and taking a filtrate to obtain a solution to be detected.
In one embodiment, the microfiltration membrane is a 0.2 μm or 0.45 μm PTFE microfiltration membrane.
In one embodiment, the sample pre-treatment is: taking a textile sample to be detected, cutting the textile sample into 2mm multiplied by 2mm, accurately weighing 1.0g (accurate to 0.1mg), placing the textile sample in a 60mL sample bottle, adding 10mL acetone, placing the sample bottle in an ultrasonic generator after plugging and sealing, carrying out ultrasonic extraction for 45min, filtering an extracting solution by using a microporous filter membrane, and taking a filtrate to obtain a solution to be detected.
In one embodiment, the external standard quantifies: accurately weighing 0.01g of dibromoneopentyl glycol standard substance, dissolving the dibromoneopentyl glycol standard substance by using acetone, fixing the volume of the dibromoneopentyl glycol standard substance into a 10mL volumetric flask, preparing 1000mg/L single-standard stock solution, diluting the single-standard stock solution by using acetone step by step to prepare 0.5mg/L, 1.0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L and 20.0mg/L dibromoneopentyl glycol standard working solution, taking the mass concentration of the dibromoneopentyl glycol standard working solution as a horizontal coordinate and the peak area of the dibromoneopentyl glycol in a chromatogram as a vertical coordinate, drawing a standard working curve, substituting the chromatographic peak area value of the dibromoneopentyl glycol in a sample to be detected measured under the same condition into the standard working curve, calculating the concentration of the dibromoneopentyl glycol, and calculating the content of the dibromoneopentyl glycol in the sample to be detected according to the concentration of the dibromoneopentyl glycol.
In one embodiment, the detection limit of the detection method is 0.045 mg/L.
In one embodiment, the relative standard deviation of the detection method is less than or equal to 3.6 percent.
In one embodiment, the assay has a spiked recovery of 99.4% to 100.7%.
The invention has the beneficial effects that: according to the invention, the dibromoneopentyl glycol is detected by adopting a gas chromatography-mass spectrometry combined technology, the detection result is high in accuracy, wherein the gas chromatography is adopted to separate the object to be detected, the separation time is short, the separation effect is good, and the mass spectrometry detector is adopted to perform qualitative detection on the object to be detected, so that the result is more accurate; the concentration of the object to be detected can be quickly obtained through a linear equation, and the accuracy is high; the detection limit of the detection method is as low as 0.045mg/L, the recovery rate is 99.4-100.7%, and the relative standard deviation is not more than 3.6%.
Drawings
Fig. 1 is a graph comparing the extraction efficiency of an extraction solvent for dibromoneopentyl glycol in textiles.
Fig. 2 is a graph of the effect of extraction time on the efficiency of extraction of dibromoneopentyl glycol from textiles.
FIG. 3 is a total ion current chromatogram of example 1.
Figure 4 is a selective ion scan chromatogram of dibromoneopentyl glycol of example 1.
Fig. 5 is a mass spectrum of dibromoneopentyl glycol of example 1.
FIG. 6 is a standard working curve for dibromoneopentyl glycol of example 1.
Fig. 7 is a total ion current chromatogram of comparative example 1.
Fig. 8 is a total ion current chromatogram of comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and the detailed description. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The information of the main instruments and experimental materials is as follows:
gas chromatography-mass spectrometer: 7890B-5977B, Agilent, USA;
an ultrasonic generator: 2300HT model, shanghai' an spectral science instruments ltd;
a chromatographic column: DB-624: 30 m.times.50 μm.times.1.40 μm, Agilent Inc., USA;
dibromo neopentyl glycol: purity 98%, Sigma-Aldrich, USA;
acetone: pure chromatography, Shanghai' an spectral science instruments Co.
Optimization of sample pretreatment conditions
The extraction solvent is one of important factors influencing the extraction efficiency of the dibromoneopentyl glycol in the textile, and the influence of the extraction solvent on the extraction efficiency of the dibromoneopentyl glycol in the textile is firstly considered in the experimental process so as to select the proper extraction solvent.
In this embodiment, four solvents, namely methanol, ethanol, ethylene glycol and acetone, are used as extraction solvents, and the influence of the extraction solvents on the recovery rate of dibromoneopentyl glycol in the textile to be tested is examined: the four solvents are selected to carry out an extraction effect comparison test on a positive sample with a known content, and the result is shown in figure 1.
As can be seen from FIG. 1, the acetone extraction is the best and the interference is less; the extraction rate of ethanol is low; the extraction efficiency of methanol and glycol is general, so acetone is selected as the extraction solvent in the embodiment.
In order to determine the appropriate extraction time, in the experiment, a sample with known positive content is taken as an object, acetone is used for carrying out ultrasonic extraction on the dibromoneopentyl glycol in the textile to be detected, the ultrasonic time is 15min, 30min, 45min, 60min, 75min and 90min, the influence of the ultrasonic time on the extraction efficiency of the bromoneopentyl glycol is examined, and the result is shown in fig. 2.
As can be seen from fig. 2, the extraction effect of dibromoneopentyl glycol is gradually improved with the increase of the extraction time, reaches the maximum when the ultrasonic time is 45min, and then becomes stable, so the optimal extraction time is 45 min.
Therefore, the optimization conditions for sample pretreatment are as follows: ultrasonic extracting with acetone as solvent for 45 min.
And detecting the dibromoneopentyl glycol in the textile according to the optimized condition of the sample pretreatment.
Example 1
In this embodiment, the method for detecting dibromoneopentyl glycol in textiles comprises the following steps:
sample pretreatment: taking a textile sample to be detected, cutting the textile sample into 2mm multiplied by 2mm, accurately weighing 1.0g, placing the textile sample into a 60mL sample bottle, accurately adding 10mL acetone, placing the sample bottle into an ultrasonic generator after plugging and sealing, ultrasonically extracting for 45min, filtering an extracting solution by using a 0.45 mu m PTFE microporous filter membrane, and taking filtrate to obtain a solution to be detected.
Gas chromatography-mass spectrometry detection: and (3) carrying out gas chromatography-mass spectrometry detection on the filtrate, and quantifying by an external standard method.
In this example, the conditions of the gas chromatography were: a chromatographic column: DB-624 capillary chromatography column: 30 m.times.250. mu.m.times.1.40 μm; temperature rising procedure: the initial temperature is 150 ℃, the temperature is kept for 1min, then the temperature is raised to 250 ℃ at the speed of 25 ℃/min, and the temperature is kept for 6 min; sample inlet temperature: 250 ℃; carrier gas: high-purity helium with purity of 99.999% and flow rate of 1.5 mL/min; sample introduction mode: no shunt sampling; injection volume 1. mu.L.
In this example, the conditions of mass spectrometry were: electron bombardment ionization, electron energy of 70eV, ion source temperature: 230 ℃; GC-MS interface temperature: 250 ℃; temperature of the quadrupole rods: 150 ℃; solvent retardation: 5 min; an acquisition mode: full scan qualitative, and selective ion scan quantitative.
In this example, the external standard quantifies: (1) preparing a standard solution of dibromoneopentyl glycol: respectively and accurately weighing 0.01g of dibromoneopentyl glycol standard substance, dissolving the dibromoneopentyl glycol standard substance by using acetone, and fixing the volume to a 10mL volumetric flask to prepare 1000mg/L single-standard stock solution. Then accurately transferring a proper amount of standard stock solution, and diluting with acetone step by step to prepare standard working solutions of 0.5mg/L, 1.0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L and 20.0 mg/L; (2) performing gas chromatography-mass spectrometry detection on the dibromoneopentyl glycol standard solution according to the chromatographic conditions and the mass spectrometry conditions, and drawing a standard working curve by taking the mass concentration of the dibromoneopentyl glycol standard solution as a horizontal coordinate and the peak area of the dibromoneopentyl glycol in the chromatogram as a vertical coordinate; (3) substituting the chromatographic peak area of the dibromo neopentyl glycol in the sample to be detected, which is measured under the same condition, into a standard working curve, calculating the concentration of the dibromo neopentyl glycol, and calculating the content of the dibromo neopentyl glycol in the sample to be detected according to the concentration of the dibromo neopentyl glycol.
FIG. 3 is a total ion current chromatogram obtained according to the above-described detection method.
The dibromoneopentyl glycol retention times and ion selection are shown in table 1.
TABLE 1 Retention time, quantitative ion and qualitative ion of dibromoneopentyl glycol
| Target object | Retention time/(min) | Quantitative ion/(m/z) | Qualitative ion/(m/z) |
| Dibromo neopentyl glycol | 7.479 | 214 | 214,133,151 |
As can be seen from table 1, under the above conditions of gas chromatography and mass spectrometry, the retention time of dibromoneopentyl glycol was short, the detection efficiency was high, the qualitative ions were 214, 133, and 151, and the quantitative ions were 214.
Fig. 4 is a selective ion scanning chromatogram of dibromoneopentyl glycol obtained according to the detection method.
Fig. 5 is a mass spectrum of dibromoneopentyl glycol obtained according to the above detection method.
Fig. 6 is a standard working curve drawn according to a standard solution in the quantification by an external standard method in this example, and the linear range, linear equation, correlation coefficient, and detection limit (MDL) of dibromoneopentyl glycol are shown in table 2, and a blank standard addition method is adopted for the determination of the detection limit.
TABLE 2 Linear relationship and detection limits for dibromoneopentyl glycol
| Target object | Linear Range (mg/L) | Linear equation of equations | Correlation coefficient | MDL(mg/L) |
| Dibromo neopentyl glycol | 0.5～20 | Y＝21090X－11980 | 0.9991 | 0.045 |
As can be seen from FIG. 6 and Table 2, the concentration of dibromoneopentyl glycol has a good linear relationship in the range of 0.5-20 mg/L, the correlation coefficient is greater than 0.9990, and the detection limit (MDL) of the method is 0.045 mg/L.
Example 2
Precision and recovery rate of detection method
The negative samples were subjected to the addition of 3 levels of 0.5mg/L, 5mg/L and 20mg/L for recovery assay, and the assay was repeated 7 times for each level of addition according to the GC-MS detection method described in example 1, with the results shown in Table 3.
Table 3 recovery and precision of dibromoneopentyl glycol spiked (n ═ 7)
| Adding quantity of scalar | Recovery/(%) | Relative standard deviation RSD/(%) |
| 0.5 | 99.4 | 3.6 |
| 5 | 100.7 | 2.6 |
| 20 | 99.7 | 1.9 |
As can be seen from Table 3, the recovery rate of the spiked samples is 99.4-100.7% and the Relative Standard Deviation (RSD) is 1.9-3.6% at the 3 spiked levels, which indicates that the detection method of the invention has good recovery rate and high precision.
Comparative example 1
Dibromoneopentyl glycol in the textile was detected by the method described in reference example 1, the procedure was essentially the same as in example 1, except that the column was changed to: rxi-5sil MS (30 m.times.0.25 mm.times.0.25 μm). The resulting total ion current chromatogram is shown in FIG. 7.
Comparative example 2
Dibromoneopentyl glycol in the textile was detected by the method described in reference example 1, the procedure was essentially the same as in example 1, except that the column was changed to: DB-5HT (15m 0.25mm 0.10 u m). The resulting total ion current chromatogram is shown in FIG. 8.
As can be seen from the comparison between FIG. 3 and FIGS. 7 and 8, the textile to be detected cannot be separated on the Rxi-5sil MS chromatographic column and the DB-5HT chromatographic column, but can be well separated on the DB-624 chromatographic column, so that the type of the chromatographic column has a great influence on the detection of the dibromoneopentyl glycol in the textile, and the detection of the dibromoneopentyl glycol in the textile can be realized only by using the DB-624 capillary chromatographic column (30m multiplied by 250 μm multiplied by 1.40 μm) provided by the invention.
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. The method for detecting dibromoneopentyl glycol in textiles is characterized by comprising the following steps:
sample pretreatment: adding acetone into a sample to be detected, carrying out ultrasonic extraction, and taking an extracting solution to obtain a solution to be detected;
gas chromatography-mass spectrometry detection: carrying out gas chromatography-mass spectrometry detection and external standard method quantification on the solution to be detected, wherein,
the conditions of the gas chromatography were: a chromatographic column: DB-624 capillary chromatography column; adopting temperature programming, wherein the temperature programming comprises the following steps: the initial temperature is 120-160 ℃, the temperature is kept for 0.5-2 min, then the temperature is increased to 230-260 ℃ at the speed of 15-30 ℃/min, the temperature is kept for 5-9 min, and the temperature of a sample inlet is 230-260 ℃; carrier gas: the flow rate is 1.2-2.0 mL/min; sample introduction mode: no flow diversion;
the mass spectrum conditions are as follows: electron bombardment ionization, ion source temperature: 200-230 ℃; gas chromatography-mass spectrometry interface temperature: 230-280 ℃; solvent delay time: 3-6 min; an acquisition mode: a full scan mode and a selective ion scan mode.
2. The detection method according to claim 1, wherein the gas chromatography is performed under the following conditions: a chromatographic column: DB-624 capillary chromatography column 30m × 250 μm × 1.40 μm; temperature rising procedure: the initial temperature is 120-160 ℃, the temperature is kept for 0.5-2 min, then the temperature is increased to 230-260 ℃ at the speed of 15-30 ℃/min, the temperature is kept for 5-9 min, and the temperature of a sample inlet is 230-260 ℃; carrier gas: high purity helium with purity > 99.999%; flow rate: 1.2-2.0 mL/min; no shunt sampling; the injection volume is 1-2 mu L.
3. The detection method according to claim 2, wherein the temperature raising program: the initial temperature is 150 deg.C, and the temperature is maintained for 1min, and then increased to 250 deg.C at a rate of 25 deg.C/min, and maintained for 6 min.
4. The detection method according to claim 1, wherein the mass spectrometry conditions are electron bombardment ionization, electron energy: 70 eV; ion source temperature: 200-230 ℃; GC-MS interface temperature: 230-280 ℃; temperature of the quadrupole rods: 150 ℃; solvent retardation: 3-6 min; ion scanning quantification was selected with full scan qualitative.
5. The detection method according to claim 4, wherein the full scan qualitatively determines the ions as 214, 133, 151 and the selected ion scan quantitatively determines the ions as 214.
6. The detection method according to claim 1, wherein the sample pretreatment is: taking a sample to be detected, shearing the sample to be detected into a size of 2-5 mm multiplied by 2-5 mm, weighing 0.5-2.0 g, adding 5-20 mL of acetone, carrying out ultrasonic extraction for 45-90 min, filtering an extracting solution by using a microporous filter membrane, and taking a filtrate to obtain a solution to be detected.
7. The detection method according to claim 6, wherein the microfiltration membrane is a 0.2 μm or 0.45 μm PTFE microfiltration membrane.
8. The assay of any one of claims 1-7, wherein the detection limit of the assay is 0.045 mg/L.
9. The assay of any one of claims 1-7, wherein the relative standard deviation of the assay is ≤ 3.6%.
10. The assay of any one of claims 1-7, wherein the assay has a normalized recovery of 99.4% to 100.7%.
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| CN113390990A (en) * | 2021-06-09 | 2021-09-14 | 谱尼测试集团股份有限公司 | Method for detecting 2, 3-dibromo-1-propanol, dibromo neopentyl glycol and tribromo neopentyl alcohol in chemical products |
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