Instrument detection method for peculiar smell substances in mulberry silk floss products

Abstract

The invention belongs to the technical field of silk detection, and particularly relates to an instrument detection method for peculiar smell substances in mulberry silk floss products. The odor source chromatographic peak of the mulberry silk floss products is found by SPME-GC / MS, the corresponding relationship between odor and specific chemicals is revealed, and a detection scheme is given. Compared with the prior art, the instrument detection method has the advantages of accurate quantification, good repeatability, high recovery rate of peculiar smell substances, reduced labor intensity ofpersonnel, low dependence on subjective judgment of professionals and the like, and operation is convenient.

Description

technical field

[0001] The invention belongs to the technical field of silk detection, and in particular relates to an instrument detection method for odorous substances in mulberry silk cotton products. Background technique

[0002] In the cocoon reeling process, because the existing technology cannot completely remove the pupa oil, the remaining pupa oil is oxidatively denatured, and the final silk fabric may produce a special, unspeakable unpleasant smell, resulting in a decline in the quality of the silk fabric and a greater loss in value. Big.

[0003] For the odor of textiles, my country currently has the following standards, including GB18401-2010 "National Basic Safety Technical Specifications for Textile Products", GB / T28024-2011 "General Technical Requirements for Fiber Products for Batting", GB / T 18885-2009 "Ecological Textile Technology Requirements" and FZ / T20027-2014 "Method for Determination of Odor of Cashmere Products", etc. These standards specify the type...

Examples

Embodiment 1

[0050] An instrument detection method for odorous substances in mulberry silk cotton products, comprising the following steps:

[0051] (1) Put 0.5g of the mulberry silk cotton product to be tested in water for 30 minutes, centrifuge and dehydrate at 10000rpm for 5 minutes, put it into an open beaker, place it at 40°C for 4 hours, and then transfer it into a headspace sampling bottle to obtain a sample bottle to be tested ;

[0052] (2) Boil 0.5g non-polluted mulberry silk cotton in boiling water for 30 minutes, dry at 120°C for 20 minutes, then place it in methanol for ultrasonic extraction for 30 minutes, dry it in the air and dry at 120°C for 20 minutes, soak in water for 30 minutes, 10000rpm Centrifuge and dehydrate for 5 minutes, put it into an open beaker, place it at 40°C for 4 hours, and then transfer it into a headspace sample bottle to obtain a blank sample bottle;

[0053] (3) Take the empty bottle, blank sample bottle, and sample bottle to be tested as the sample ...

Embodiment 2

[0062] (1) Boil five 0.50g non-polluting mulberry silk cotton products in boiling water for 30 minutes, dry them at 120°C for 20 minutes, then place them in methanol for ultrasonic extraction for 30 minutes, dry them in the air and dry them at 120°C for 20 minutes; then soak them in water , After centrifugation and dehydration, place at 40°C for 240 minutes, and then put them into headspace sampling vials respectively to obtain five blank vials;

[0063] (2) Dilute the 1,2-dimethylhydrazine (CAS No: 540-73-8) standard with methanol to obtain standard working solutions with different concentrations, 10μg / mL, 50μg / mL, 200μg / mL, 500μg / mL, 1000μg / mL; 5μL of the standard working solution was injected into each blank vial using a micro syringe to obtain a standard working solution vial, and the concentration of 1,2-dimethylhydrazine in the standard working solution vial was 0.1 mg / kg, 0.5mg / kg, 2mg / kg, 5mg / kg, 10mg / kg;

[0064] (3) Using the empty bottle, blank sample bottle, and ...

Embodiment 3

[0066] According to the method of Example 2, standard working solution sample vials were prepared, in which the concentrations of 1,2-dimethylhydrazine were 1 mg / kg, 5 mg / kg and 50 mg / kg, respectively.

[0067] Take the empty bottle, blank sample bottle, and standard working solution sample bottle as the sampling bottle in turn, and use headspace solid phase microextraction-gas chromatography-mass spectrometry to measure the blank sample chromatogram and standard working curve chromatogram, according to 1,2 -The mass spectrogram, retention time and response value thereof of dimethylhydrazine, obtain mass spectrometry response value, measure 6 times for every sample, then calculate average recovery rate and relative standard deviation, bring into mass spectrometry response value-concentration standard working curve, obtain 1 , the detection concentration of 2-dimethylhydrazine, the results are shown in Table 1, the recoveries of 6 parallel samples of all the levels of addition a...

technical field

[0001] The invention belongs to the technical field of silk detection, and in particular relates to an instrument detection method for odorous substances in mulberry silk cotton products. Background technique

[0002] In the cocoon reeling process, because the existing technology cannot completely remove the pupa oil, the remaining pupa oil is oxidatively denatured, and the final silk fabric may produce a special, unspeakable unpleasant smell, resulting in a decline in the quality of the silk fabric and a greater loss in value. Big.

[0003] For the odor of textiles, my country currently has the following standards, including GB18401-2010 "National Basic Safety Technical Specifications for Textile Products", GB / T28024-2011 "General Technical Requirements for Fiber Products for Batting", GB / T 18885-2009 "Ecological Textile Technology Requirements" and FZ / T20027-2014 "Method for Determination of Odor of Cashmere Products", etc. These standards specify the type...

Examples

Embodiment 1

[0050] An instrument detection method for odorous substances in mulberry silk cotton products, comprising the following steps:

[0051] (1) Put 0.5g of the mulberry silk cotton product to be tested in water for 30 minutes, centrifuge and dehydrate at 10000rpm for 5 minutes, put it into an open beaker, place it at 40°C for 4 hours, and then transfer it into a headspace sampling bottle to obtain a sample bottle to be tested ;

[0052] (2) Boil 0.5g non-polluted mulberry silk cotton in boiling water for 30 minutes, dry at 120°C for 20 minutes, then place it in methanol for ultrasonic extraction for 30 minutes, dry it in the air and dry at 120°C for 20 minutes, soak in water for 30 minutes, 10000rpm Centrifuge and dehydrate for 5 minutes, put it into an open beaker, place it at 40°C for 4 hours, and then transfer it into a headspace sample bottle to obtain a blank sample bottle;

[0053] (3) Take the empty bottle, blank sample bottle, and sample bottle to be tested as the sample ...

Embodiment 2

[0062] (1) Boil five 0.50g non-polluting mulberry silk cotton products in boiling water for 30 minutes, dry them at 120°C for 20 minutes, then place them in methanol for ultrasonic extraction for 30 minutes, dry them in the air and dry them at 120°C for 20 minutes; then soak them in water , After centrifugation and dehydration, place at 40°C for 240 minutes, and then put them into headspace sampling vials respectively to obtain five blank vials;

[0063] (2) Dilute the 1,2-dimethylhydrazine (CAS No: 540-73-8) standard with methanol to obtain standard working solutions with different concentrations, 10μg / mL, 50μg / mL, 200μg / mL, 500μg / mL, 1000μg / mL; 5μL of the standard working solution was injected into each blank vial using a micro syringe to obtain a standard working solution vial, and the concentration of 1,2-dimethylhydrazine in the standard working solution vial was 0.1 mg / kg, 0.5mg / kg, 2mg / kg, 5mg / kg, 10mg / kg;

[0064] (3) Using the empty bottle, blank sample bottle, and ...

Embodiment 3

[0066] According to the method of Example 2, standard working solution sample vials were prepared, in which the concentrations of 1,2-dimethylhydrazine were 1 mg / kg, 5 mg / kg and 50 mg / kg, respectively.

[0067] Take the empty bottle, blank sample bottle, and standard working solution sample bottle as the sampling bottle in turn, and use headspace solid phase microextraction-gas chromatography-mass spectrometry to measure the blank sample chromatogram and standard working curve chromatogram, according to 1,2 -The mass spectrogram, retention time and response value thereof of dimethylhydrazine, obtain mass spectrometry response value, measure 6 times for every sample, then calculate average recovery rate and relative standard deviation, bring into mass spectrometry response value-concentration standard working curve, obtain 1 , the detection concentration of 2-dimethylhydrazine, the results are shown in Table 1, the recoveries of 6 parallel samples of all the levels of addition a...

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