CN111624268A - Method for detecting peculiar smell compounds in textiles - Google Patents

Abstract

The invention discloses a method for detecting odor compounds in textiles, which comprises the following steps: (1) weighing a number of shredded and mixed textile samples and placing them in a headspace bottle; (2) adopting solid-phase microextraction The sample injection method was analyzed by gas chromatography-mass spectrometer; (3) the contents of 13 odor compounds in textiles were qualitatively and quantitatively calculated according to the retention times and corresponding peak areas of 13 odor compounds. The method of the invention can simultaneously detect whether 13 kinds of odor compounds are contained in textiles, without pretreatment, without organic solvent recontamination, combined with gas mass spectrometry trace analysis technology, can realize accurate qualitative and quantitative testing of odor target substances, and reduce false positives. The possibility of a judgment can provide an objective evaluation for the arbitration inspection, supervision and random inspection of textiles.

Description

A detection method for odor compounds in textiles

technical field

The invention relates to the field of textile detection, in particular to a detection method for odor compounds in textiles.

Background technique

Odor substances are mainly derived from a large amount of waste gas generated in the process of human life and industrial and agricultural production. In addition to bringing people uncomfortable feeling, they can also cause harm to health and ecological environment in severe cases. At present, odor pollution has been highly valued by countries all over the world and listed as one of the seven major environmental hazards. Among them, textile odor is closely related to people's daily life. Since the "poisonous school uniform" incident in 2013, the safety of textiles has always been a national and national issue. industry focus. At present, the detection and evaluation of textile odor is carried out by professionals using olfactory discrimination, such as the odor detection in my country's mandatory standard GB 18401-2010 "National Textile Products Basic Safety Technical Specifications", but this subjective evaluation method is not stable. It is not only impossible to accurately quantify the degree of odor, but also some of the compounds in the odor are harmful substances to the human body, which poses a certain threat to the health of the inspectors. Therefore, textile odor assessment needs to explore a new objective assessment method. There are two common objective detection methods for odor in previous studies: electronic nose and headspace-gas chromatography-mass spectrometry. Electronic nose is a gas detector imitating biological nose, which belongs to the combination product of instrumental analysis method and sensory evaluation method. Electronic nose is a non-destructive analysis technology that is simple, fast, and applicable to a wide range of samples. However, the sensor array in the system has poor specificity and stability, and is easily affected by environmental factors. In addition, the sensor is easily overloaded or poisoned, and reacts with interfering gases. affect the measurement results. Headspace technology is a commonly used technique in the qualitative and quantitative analysis of complex odor pollutants. This method can effectively separate mixtures and determine the chemical concentration of each component in odor samples. With the blessing of tandem mass spectrometry, the detection of odor compounds can be further improved. limit and sensitivity. For the detection of odor compounds in textiles, my country has not yet had a clear and unified standard, and the market is chaotic, which brings difficulties to the government's market supervision. Therefore, how to qualitatively and quantitatively detect odor compounds in textiles and establish a fast, effective and objective detection method to protect the rights and interests of consumers has become an urgent problem to be solved.

SUMMARY OF THE INVENTION

Aiming at the deficiencies of the existing detection methods, the present invention provides a detection method for odor compounds in textiles, which can measure the content of 13 odor compounds (see Table 1) contained in textiles.

The technical scheme of the present invention is:

A method for detecting odor compounds in textiles is characterized in that the content of odor compounds in textiles is determined by using solid-phase microextraction to inject samples, and gas chromatography-mass spectrometry.

More specifically, a method for detecting odorous compounds in textiles of the present invention is characterized in that it includes the following steps: (1) weighing a number of mass of shredded and mixed textile samples and placing them in a headspace bottle; ( 2) The solid-phase microextraction injection method was used for analysis by gas chromatography-mass spectrometer; (3) the content of 13 odor compounds in textiles was qualitatively and quantitatively calculated according to the retention times and corresponding peak areas of 13 odor compounds;

The mass of the textile sample is 1-2g;

The solid-phase microextraction conditions are as follows: the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), the coating thickness of the extraction head is 50/30 μm; the equilibration time is 15 ~20min; extraction time is 15~25min; desorption time is 2~5min;

The analysis conditions of the gas chromatography-mass spectrometer are: the chromatographic column is a polyethylene glycol capillary column, such as an AgilentDB-WAX capillary column or other capillary columns of the same polarity; the carrier gas is helium; the column flow rate is 1.5-2 mL/min ; Injection port temperature 230-250°C; split injection, split ratio of (5-10): 1; temperature programmed: initial temperature 30-50°C, maintained for 4-6min, heated to 10-20°C/min 240～260℃, hold for 10～15min; EI: 70eV, ion source temperature 200～230℃, interface temperature 240～260℃, mass scanning range is 25～250amu;

The content of 13 odor compounds in textile samples was calculated as follows:

Xi=(Ai×Ci×V)/(Ais×m) (1)

Wherein: Xi is the content of odor compound i in the tested sample (μg/g);

Ai is the peak area of odor compound i in the detected sample;

Ci is the mass concentration of odor compound i in the standard solution (μg/mL);

V is the standard solution added volume (mL);

m is the sample size (g) of the shredded textile sample;

Ais is the peak area of odor compound i in the standard solution.

Table 1 Characteristic ions and odor descriptions of 13 odor compounds

In a method for detecting odor compounds in textiles of the present invention, the characteristic ions and odor descriptions of 13 odor compounds are shown in Table 1.

Compared with the prior art, the detection method of the present invention can simultaneously detect whether 13 kinds of odor compounds are contained in textiles, which provides a new idea for the odor test of textiles, without pretreatment, without organic solvent recontamination, and combined with gas mass spectrometry trace analysis. The technology can accurately calculate the content of various odor compounds and achieve accurate qualitative and quantitative testing of odor targets; compared with the odor detection method, the analyst's experience requirements are greatly reduced, and the possibility of misjudgment is greatly reduced. , to provide objective evaluation for arbitration inspection, supervision and random inspection of textiles.

Description of drawings

Fig. 1 is the selected ion chromatogram of standard solution;

In the picture: 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-n-tetradecane, 12-n-pentadecane, 13-n-hexadecane.

FIG. 2 is a sample selected ion chromatogram of Example 1. FIG.

FIG. 3 is a sample selected ion chromatogram of Example 2. FIG.

Detailed ways

The present invention will be further described below in conjunction with specific embodiments. It should be understood that this embodiment is only used to illustrate the present invention and not to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Example 1

(1) Take a gray textile sample, cut it into pieces, mix it, weigh 1 g of the sample, and place it in a headspace bottle;

(2) Prepare mixed standard working solution: dilute the mixed standard stock solution into a mixed standard working solution with a concentration of 20 μg/mL;

(3) The gas chromatography-mass spectrometer (GC-MS) conditions are as follows, the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), and the coating thickness of the extraction head is; 50 The equilibration time is 15min; the extraction time is 20min; the desorption time is 2min; the analysis conditions of the gas chromatography-mass spectrometer are: the chromatographic column is a DB-WAX capillary column; the carrier gas is helium; the column flow rate is 1.5mL/min ; Inlet temperature 250°C; split injection, split ratio of 5:1; temperature program: initial temperature 40°C, maintained for 5min, heated to 250°C at 15°C/min, maintained for 15min; EI: 70eV, ion source The temperature is 230℃, the interface temperature is 260℃, and the mass scanning range is 25～250amu.

The selected ion chromatogram of the standard solution is shown in Figure 1. The peaks in the figure are completely separated, and the peaks of each spectrum are sharp and symmetrical. It can be shown that the selected characteristic target ion has high sensitivity, good selectivity, less interference, wide linear range, accurate qualitative and low quantification limit. The selected ion chromatogram of the sample is shown in Figure 2.

The aniline peak appears at the same retention time of 9.93min between the sample to be tested and the standard reference sample. The linear equation of the aniline peak is: y=4.31344×10 ⁶ x (y is the peak area, x is the content, the unit is mg/kg, linear The correlation coefficient R ² =0.9961, the lower limit of determination is 0.08 mg/kg), and the content of aniline, an odorous compound in the textile sample, is calculated as: 15 mg/kg.

Example 2

(1) Take a white textile sample, cut it into pieces and mix it, weigh 1 g of the sample, and place it in a headspace bottle;

(2) Prepare mixed standard working solution: dilute the mixed standard stock solution into a mixed standard working solution with a concentration of 20 μg/mL;

(3) The gas chromatography-mass spectrometer (GC-MS) conditions are as follows, and the solid-phase microextraction conditions are: the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS), and the extraction head is The thickness of the head coating was 50/30 μm; the equilibration time was 20 min; the extraction time was 25 min; and the desorption time was 5 min. The analysis conditions of the gas chromatography-mass spectrometer were as follows: the chromatographic column was a DB-WAX capillary column; the carrier gas was helium; the column flow rate was 2 mL/min; the inlet temperature was 250 °C; Program temperature: the initial temperature is 40 °C, maintained for 5 min, and the temperature is increased to 250 °C at 10 °C/min, and maintained for 10 min; EI: 70 eV, ion source temperature 230 °C, interface temperature 250 °C, mass scanning range is 25 ~ 250amu.

The selected ion chromatogram of the standard solution is shown in Figure 1, and the selected ion chromatogram of the sample is shown in Figure 3. At the same retention time of 17.08min, the sample to be tested and the standard reference sample have an earthy element peak. The linear equation of earth element peak is: y=5.48916×10 ⁵ x (y is the peak area, x is the content, and the unit is mg /kg, the linear correlation coefficient R ² =0.9954, the lower limit of determination is 0.10mg/kg), the odor compound in the textile sample is calculated by the formula, and its content is: 0.5mg/kg.

Claims (6)

1. a detection method for peculiar smell compounds in textiles, is characterized in that, adopts solid-phase microextraction to inject sample, and gas chromatography-mass spectrometry is used to measure the content of peculiar smell compounds in textiles. 2. The method for detecting odor compounds in textiles according to claim 1, characterized in that it comprises the following steps: (1) weighing a number of mass of the shredded and mixed textile samples and placing them in a headspace bottle; ( 2) The solid-phase microextraction method was used for sample injection, and gas chromatography-mass spectrometer was used for analysis; (3) The contents of 13 odor compounds in textiles were qualitatively and quantitatively calculated according to the retention times and corresponding peak areas of 13 odor compounds. 3 . The method for detecting odor compounds in textiles according to claim 2 , wherein the mass of the textile sample is 1-2 g. 4 . 4. The method for detecting odor compounds in textiles according to claim 2, wherein the solid-phase microextraction conditions are: the extraction head is divinylbenzene/carbon molecular sieve/polydimethylsiloxane ( DVB/CAR/PDMS), the coating thickness of the extraction head is 50/30 μm; the equilibration time is 15-20 min; the extraction time is 15-25 min; and the desorption time is 2-5 min. 5. the detection method of peculiar smell compound in textile according to claim 2 is characterized in that, the analysis condition of gas chromatography-mass spectrometer is: chromatographic column is polyethylene glycol capillary chromatographic column, for example: Agilent DB-WAX capillary chromatograph Column or other equivalent polar capillary column; the carrier gas is helium; the column flow rate is 1.5～2mL/min; the inlet temperature is 230～250℃; The initial temperature is 30～50℃, maintained for 4～6min, the temperature is increased to 240～260℃ at 10～20℃/min, and kept for 10～15min; EI: 70 eV, ion source temperature 200～230℃, interface temperature 240～260 ℃, the mass scanning range is 25～250amu. 6. The detection method of peculiar smell compounds in textiles according to claim 2, is characterized in that, the content of 13 kinds of peculiar smell compounds in the textile sample is calculated as follows: Xi=(Ai×Ci×V)/(Ais×m) (1) Wherein: Xi is the content of the odor compound i in the tested sample (μg/g); Ai is the peak area of odor compound i in the detected sample; Ci is the mass concentration of odor compound i in the standard solution (μg/mL); V is the standard solution added volume (mL); m is the sample size (g) of the shredded textile sample; Ais is the peak area of odor compound i in the standard solution.

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