CN111624268A - Method for detecting peculiar smell compounds in textiles - Google Patents
Method for detecting peculiar smell compounds in textiles Download PDFInfo
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- CN111624268A CN111624268A CN202010365324.0A CN202010365324A CN111624268A CN 111624268 A CN111624268 A CN 111624268A CN 202010365324 A CN202010365324 A CN 202010365324A CN 111624268 A CN111624268 A CN 111624268A
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Abstract
The invention discloses a method for detecting peculiar smell compounds in textiles, which comprises the following steps: (1) weighing a plurality of sheared and uniformly mixed textile samples by mass, and placing the textile samples into a headspace bottle; (2) analyzing by a gas chromatography-mass spectrometer in a solid phase microextraction sample injection mode; (3) and qualitatively and quantitatively calculating the contents of the 13 odor compounds in the textile according to the retention time of the 13 odor compounds and the corresponding peak areas. The method can simultaneously detect whether the textile contains 13 peculiar smell compounds, does not need pretreatment, does not have organic solvent recontamination, can realize accurate qualitative and quantitative test on peculiar smell target substances by combining a gas phase mass spectrum trace analysis technology, reduces the possibility of misjudgment, and provides objective evaluation for arbitration inspection and supervision spot check of the textile.
Description
Technical Field
The invention relates to the field of textile detection, in particular to a method for detecting peculiar smell compounds in textiles.
Background
The peculiar smell substances mainly come from a large amount of waste gas generated in the processes of human life and industrial and agricultural production, which not only brings discomfort to people, but also causes harm to the health and the ecological environment in severe cases. At present, peculiar smell pollution is highly valued by countries in the world and is listed as one of seven public hazards of the environment, wherein peculiar smell of textiles is closely related to daily life of people, and since the occurrence of a toxic school uniform event in 2013, the safety problem of the textiles is always the key point of national and industrial attention. At present, the detection and evaluation of textile odor are carried out by a smell discrimination method by professional personnel, such as odor detection in national mandatory standard GB 18401-2010 national basic safety technical Specification for textile products, but the subjective evaluation method has low stability and is greatly influenced by human factors, so that the odor degree cannot be accurately quantified, and compounds in part of the odor are substances harmful to human bodies, thereby causing certain threat to the body health of inspectors. Therefore, there is a need to explore a new objective evaluation method for textile odor evaluation. In previous studies, two methods are common for objective detection of odor: an electronic nose and a headspace-gas chromatography-mass spectrometry combined method. The electronic nose is a gas detector simulating biological nose, and belongs to the combined product of instrument analysis method and sensory evaluation method. The electronic nose is a nondestructive analysis technology with simple and rapid operation and wide sample application range, but the sensor array in the system has poor specificity and stability and is easily influenced by environmental factors, and in addition, the sensor is easily overloaded or poisoned and reacts with interference gas to influence the measurement result. The headspace technology is a commonly used technology in qualitative and quantitative analysis of complex odor pollutants, the method effectively separates a mixture and measures the chemical concentration of each component in an odor sample, and if the mixture is supported by a tandem mass spectrum, the detection limit and the sensitivity of the odor compound can be further improved. For the detection of peculiar smell compounds in textiles, at present, China has no clear and unified standard, the market is disordered, and the difficulty is brought to the government market supervision. Therefore, how to qualitatively and quantitatively detect the odor compounds in the textiles and establish a quick, effective and objective detection method to guarantee the rights of consumers becomes a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the existing detection method, the invention provides the method for detecting the odor compounds in the textile, which can be used for measuring the contents of 13 odor compounds (shown in table 1) contained in the textile.
The technical scheme of the invention is as follows:
the method for detecting the odor compounds in the textiles is characterized in that the content of the odor compounds in the textiles is determined by adopting a solid phase microextraction sample injection and gas chromatography-mass spectrometry combined method.
More specifically, the invention relates to a method for detecting an odor compound in a textile, which is characterized by comprising the following steps: (1) weighing a plurality of sheared and uniformly mixed textile samples by mass, and placing the textile samples into a headspace bottle; (2) analyzing by a gas chromatography-mass spectrometer in a solid phase microextraction sample injection mode; (3) qualitatively and quantitatively calculating the contents of the 13 odor compounds in the textile according to the retention time of the 13 odor compounds and the corresponding peak areas;
the mass of the textile sample is 1-2 g;
the solid phase micro-extraction conditions are as follows: the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), and the thickness of the coating of the extraction head is 50/30 μm; the balance time is 15-20 min; the extraction time is 15-25 min; the desorption time is 2-5 min;
the analysis conditions of the gas chromatography-mass spectrometer are as follows: the chromatographic column is a polyethylene glycol capillary chromatographic column, for example: an AgilentDB-WAX capillary chromatographic column or other equivalent polarity capillary column; the carrier gas is helium; the flow rate of the column is 1.5-2 mL/min; the temperature of a sample inlet is 230-250 ℃; split-flow sample injection, wherein the split-flow ratio is (5-10): 1; temperature programming: the initial temperature is 30-50 ℃, the temperature is maintained for 4-6 min, the temperature is increased to 240-260 ℃ at the speed of 10-20 ℃/min, and the temperature is maintained for 10-15 min; EI: 70eV, the ion source temperature is 200-230 ℃, the interface temperature is 240-260 ℃, and the mass scanning range is 25-250 amu;
the content of 13 off-flavor compounds in the textile sample was calculated as follows:
Xi＝(Ai×Ci×V)/(Ais×m) (1)
wherein: xi is the content (mu g/g) of the odor compound i in the detected sample;
ai is the peak area of the peculiar smell compound i in the detected sample;
ci is the mass concentration (mu g/mL) of the off-flavor compound i in the standard solution;
v is standard solution addition volume (mL);
m is the sample size (g) of the textile sample that is sheared;
ais is the peak area of the odorous compound i in the standard solution.
TABLE 113 characterization of ion and odor profiles for the odorous Compounds
In the method for detecting the odor compounds in the textile, the characteristic ions and the odor of 13 odor compounds are described in table 1.
Compared with the prior art, the detection method can simultaneously detect whether the textile contains 13 peculiar smell compounds, provides a new idea for the peculiar smell test of the textile, does not need pretreatment, does not have organic solvent recontamination, and can accurately calculate the content of each peculiar smell compound by combining a gas phase mass spectrum trace analysis technology, thereby realizing accurate qualitative and quantitative test of peculiar smell target substances; compared with the peculiar smell distinguishing method, the method has the advantages that the requirement on the working experience of an analyst is greatly reduced, the possibility of misjudgment is greatly reduced, and objective evaluation is provided for arbitration inspection and supervision spot check of textiles.
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FIG. 1 is a selective ion chromatogram of a standard solution;
in the figure: 1-methyl acrylate, 2-isooctane, 3-ethyl acrylate, 4-butyl acrylate, 5-aniline, 6-n-decane, 7-n-undecane, 8-n-dodecane, 9-n-tridecane, 10-n-tetradecane, 11-oxytetracycline, 12-n-pentadecane, 13-n-hexadecane.
FIG. 2 is a sample selective ion chromatogram of example 1.
FIG. 3 is a sample selective ion chromatogram of example 2.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that this example is for illustrative purposes only and is not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Taking a gray textile sample, shearing the gray textile sample, uniformly mixing, weighing 1g of sample, and placing the sample in a headspace bottle;
(2) preparing a mixed standard working solution: diluting the mixed standard stock solution into a mixed standard working solution with the concentration of 20 mug/mL;
(3) the gas chromatography-mass spectrometer (GC-MS) conditions were as follows, the extraction head was divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), and the thickness of the extraction head coating was; 50/30 μm; the balance time is 15 min; the extraction time is 20 min; the desorption time is 2 min; the analysis conditions of the gas chromatography-mass spectrometer are as follows: the chromatographic column is a DB-WAX capillary chromatographic column; the carrier gas is helium; the column flow rate is 1.5 mL/min; the temperature of a sample inlet is 250 ℃; split-flow sample injection, the split-flow ratio is 5: 1; temperature programming: the initial temperature is 40 ℃, the temperature is maintained for 5min, the temperature is increased to 250 ℃ at the speed of 15 ℃/min, and the temperature is maintained for 15 min; EI: 70eV, the ion source temperature is 230 ℃, the interface temperature is 260 ℃, and the mass scanning range is 25-250 amu.
The selective ion chromatogram of the standard solution is shown in figure 1, wherein the peaks are completely separated, and the peaks are sharp and have good symmetry. Therefore, the selected characteristic target ions have the advantages of high sensitivity, good selectivity, less interference, wide linear range, accurate qualitative determination and low quantitative limit. The selective ion chromatogram of the sample is shown in FIG. 2.
The sample to be tested and the standard reference sample have aniline peaks at the same retention time of 9.93min, and the linear equation of the aniline peaks is that y is 4.31344 × 106x (y is peak area, x is content, unit is mg/kg, linear correlation coefficient R2The lower limit of the measurement was 0.99618mg/kg), calculating the content of the odor compound aniline in the textile sample as follows: 15 mg/kg.
Example 2
(1) Taking a white textile sample, shearing the white textile sample, uniformly mixing, weighing 1g of the sample, and placing the sample in a headspace bottle;
(2) preparing a mixed standard working solution: diluting the mixed standard stock solution into a mixed standard working solution with the concentration of 20 mug/mL;
(3) the gas chromatography-mass spectrometer (GC-MS) conditions were as follows, and the solid phase microextraction conditions were: the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), and the thickness of the extraction head coating is as follows; 50/30 μm; the balance time is 20 min; the extraction time is 25 min; the desorption time was 5 min. The analysis conditions of the gas chromatography-mass spectrometer are as follows: the chromatographic column is a DB-WAX capillary chromatographic column; the carrier gas is helium; the column flow rate is 2 mL/min; the temperature of a sample inlet is 250 ℃; split-flow sample injection, the split-flow ratio is 7: 1; temperature programming: the initial temperature is 40 ℃, the temperature is maintained for 5min, the temperature is increased to 250 ℃ at the speed of 10 ℃/min, and the temperature is maintained for 10 min; EI: 70eV, the ion source temperature is 230 ℃, the interface temperature is 250 ℃, and the mass scanning range is 25-250 amu.
The selective ion chromatogram of the standard solution is shown in figure 1, the selective ion chromatogram of the sample is shown in figure 3, the sample to be tested and the standard reference sample have an oxytetracycline peak at the same retention time of 17.08min, and the linear equation of the oxytetracycline peak is that y is 5.48916 × 105x (y is peak area, x is content, unit is mg/kg, linear correlation coefficient R20.9954, the lower limit of the determination is 0.10mg/kg), and the odor compound in the textile sample is obtained by calculation according to a formula, wherein the content of the odor compound is as follows: 0.5 mg/kg.
Claims (6)
1. The method for detecting the odor compounds in the textiles is characterized in that the content of the odor compounds in the textiles is determined by adopting a solid phase microextraction sample injection and gas chromatography-mass spectrometry combined method.
2. The method of detecting an off-flavor compound in a textile of claim 1, comprising the steps of: (1) weighing a plurality of sheared and uniformly mixed textile samples by mass, and placing the textile samples into a headspace bottle; (2) analyzing by a gas chromatography-mass spectrometer in a solid phase microextraction sample injection mode; (3) and qualitatively and quantitatively calculating the contents of the 13 odor compounds in the textile according to the retention time of the 13 odor compounds and the corresponding peak areas.
3. The method for detecting the odor compounds in the textile according to claim 2, wherein the mass of the textile sample is 1-2 g.
4. The method for detecting the odor compounds in the textile according to claim 2, wherein the solid phase micro-extraction conditions are as follows: the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), and the thickness of the coating of the extraction head is 50/30 μm; the balance time is 15-20 min; the extraction time is 15-25 min; the desorption time is 2-5 min.
5. The method for detecting the odor compounds in the textile according to claim 2, wherein the analysis conditions of the gas chromatography-mass spectrometer are as follows: the chromatographic column is a polyethylene glycol capillary chromatographic column, for example: agilent DB-WAX capillary chromatographic column or other equivalent polarity capillary column; the carrier gas is helium; the flow rate of the column is 1.5-2 mL/min; the temperature of a sample inlet is 230-250 ℃; split-flow sample injection, wherein the split-flow ratio is (5-10): 1; temperature programming: the initial temperature is 30-50 ℃, the temperature is maintained for 4-6 min, the temperature is increased to 240-260 ℃ at the speed of 10-20 ℃/min, and the temperature is maintained for 10-15 min; EI: 70eV, 200-230 ℃ of ion source temperature, 240-260 ℃ of interface temperature and 25-250 amu of mass scanning range.
6. The method for detecting malodorous compounds in textiles of claim 2, wherein the content of 13 malodorous compounds in a textile sample is calculated as follows:
Xi=（Ai×Ci×V）/（Ais×m） （1）
wherein: xi is the content (mu g/g) of the odor compound i in the detected sample;
ai is the peak area of the peculiar smell compound i in the detected sample;
ci is the mass concentration (mu g/mL) of the off-flavor compound i in the standard solution;
v is standard solution addition volume (mL);
m is the sample size (g) of the textile sample that is sheared;
ais is the peak area of the odorous compound i in the standard solution.
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| CN114894932A (en) * | 2022-05-07 | 2022-08-12 | 安徽工程大学 | Method for detecting trace amount peculiar smell gas components in automobile textile fabric |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114894932A (en) * | 2022-05-07 | 2022-08-12 | 安徽工程大学 | Method for detecting trace amount peculiar smell gas components in automobile textile fabric |
| CN114894932B (en) * | 2022-05-07 | 2023-08-01 | 安徽工程大学 | Method for detecting trace odor components in textile fabric for automobile |
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