CN112782321A

CN112782321A - Determination method for rapidly detecting content of vitamin E in textiles

Info

Publication number: CN112782321A
Application number: CN202110256418.9A
Authority: CN
Inventors: 韩莹莹; 谭玉静; 曹石淼; 林圣光; 赵海浪; 庄园园
Original assignee: Shanghai Institute of Quality Inspection and Technical Research
Current assignee: Shanghai Institute of Quality Inspection and Technical Research
Priority date: 2021-03-09
Filing date: 2021-03-09
Publication date: 2021-05-11

Abstract

The invention provides a method for rapidly detecting the content of vitamin E in textiles, which comprises the steps of extracting a textile sample by absolute ethyl alcohol, filtering an extraction liquid to obtain a pretreatment test solution; and determining the content of the vitamin E in the liquid to be tested by adopting a high performance liquid chromatograph. The method disclosed by the invention is simple to operate, high in sensitivity, good in linear relation within the range of 2.0-100.0 mu g/mL, more than 0.999 of linear correlation coefficient and 0.05mg/kg of detection limit.

Description

Determination method for rapidly detecting content of vitamin E in textiles

Technical Field

The invention belongs to the technical field of textile detection, and particularly relates to a determination method for rapidly detecting the content of vitamin E in a textile.

Background

The textile fiber is one of the main raw materials in the textile industry, and has very important significance for the development of the textile industry. In recent years, people have increasingly raised awareness of their health care, and along with the development of industry, environmental pollution is serious, and carbon dioxide, nitrogen oxide and sulfur oxide in the atmosphere are increasing, and these pollutants have a great influence on the human body and can cause allergy to the human skin, so that it is very necessary to maintain the skin health. The skin care mode adopts cosmetics and skin care finishing clothing fabric which is in direct contact with a human body as a skin protection barrier, and is a safe and effective protection means, so that the skin care function finishing draws attention, and the skin care fiber is produced at the same time.

The skin care fiber not only has the mechanical property of common fiber, but also has the effect of beautifying and protecting skin. The skin care fiber is prepared by finishing additives with skin care functional components on the fiber by a processing and finishing technology. The textile prepared by adopting the skin care fiber has the functions of wearability and beauty and skin care. The skin care fiber and the textile thereof have the following three characteristics: (1) the nature is as follows: the raw materials are derived from natural raw material extracts, and are mild to skin; (2) health: has the effects of moistening and adjusting humidity, and is particularly suitable for fabrics such as knitted underwear and the like; (3) safety: endows the fabric with skin care and conditioning functions, and is harmless to human bodies and the environment.

Many research and development institutions at home and abroad apply high and new technology for functional finishing to fibers or fabrics, and a series of skin-care and face-beautifying fibers and textiles are continuously developed, for example, vitamin E fabrics are one of the skin-care and face-beautifying textile fibers.

Vitamin E, called VE for short, is a common medicine and a nutritional health product, and has the physiological functions of obvious antioxidation, elimination of free radicals in vivo and the like. VE is arranged on the textile by a certain method to prepare the nutritional textile with the vitamin E slow-release function, so that the application field of the vitamin E can be widened, the added value of the product is improved, the healthy life concept of modern consumers is conformed, and the requirement of people on the textile with the health care function is met, therefore, the VE textile is deeply welcomed by many people paying attention to health and beauty. In recent years, many companies and research institutions at home and abroad begin to research that vitamin E is added into fibers or is finished on textiles in a microcapsule form to produce the textiles containing the vitamin E, and the textiles can supplement the vitamin E for people at any time and any place and have the effects of whitening, moisturizing, delaying senescence and the like. The companies of Langshan (Japan) chemistry, Japan Fuji textile, Japan Rice field fiber, Jieshuang in China, Germany Dessida, etc. have achieved certain achievements in the aspects of vitamin skin care finishing agents, vitamin fibers and textile development. The company Unitika, Japan, produced Activait series products by making vitamin E into sustained-release microcapsules and attaching the microcapsules to fibers, and proposed tight-fitting garments made of such materials. At present, a lot of reports about vitamin E fibers and textiles are reported at home and abroad, and a lot of products are sold in the market, but the research reports about the detection of active ingredients in the fibers and the textiles are very few.

The appearance of the vitamin E skin care fiber is a breakthrough in the textile industry and the cosmetic industry, the vitamin E skin care fiber and the textile thereof arouse great interest of consumers, the vitamin E skin care fiber and the textile thereof become a new hot spot in textile market competition, and the development consciousness of enterprises is stimulated by the functionality and the high added value of the vitamin E skin care fiber. But counterfeit products are in the row due to the lack of detection methods and associated standards, seriously compromising consumer interest. In order to help enterprises to enhance product quality control, improve product quality and guarantee use safety of consumers, and meanwhile, in order to help the industry to standardize market order of vitamin E fabrics and promote healthy development of vitamin E skin-care fabric industry, the research on the detection method of the vitamin E content in the textile has important practical significance.

Disclosure of Invention

The invention aims to provide a scientific, reasonable, simple and rapid determination method for detecting the content of vitamin E in textiles.

The technical scheme of the invention is as follows:

the invention relates to a method for rapidly detecting the content of vitamin E in textiles, which is characterized in that a textile sample is extracted by absolute ethyl alcohol, and extract liquor is filtered to obtain pretreatment test solution; and determining the content of the vitamin E in the liquid to be tested by adopting a high performance liquid chromatograph.

More specifically, the invention discloses a method for rapidly detecting the content of vitamin E in textiles, which is characterized by comprising the following steps:

(1) sample treatment: adding absolute ethyl alcohol into a proper amount of sample, carrying out ultrasonic extraction for 10-50 min, filtering the extract by using a microporous filter membrane with the pore diameter of 0.20-0.45 mu m, and taking the filtrate as a to-be-tested solution;

(2) sample detection: injecting the liquid to be tested into a high performance liquid chromatograph to measure vitamin E and the peak area thereof, calculating the content of the vitamin E in the liquid to be tested according to a standard curve equation, and calculating the content of the vitamin E in the sample;

the sample is a piece obtained by shearing a textile sample into pieces with the size not larger than 5mm multiplied by 5 mm;

the testing conditions of the high performance liquid chromatograph are as follows: the chromatographic column is Agilent eclipse XDB C18 or equivalent chromatographic column, 4.6X150mm, 5 μm; column temperature: 20-40 ℃; sample introduction amount: 5-30 mu L; the mobile phase consists of methanol and water, the volume ratio of the methanol to the water is (99-90) to (1-10), and the flow rate of the mobile phase is 0.8-1.5 mL/min; the detector is an FLD fluorescence detector, and the detection conditions are as follows: the excitation wavelength is 290 nm-300 nm, and the emission wavelength is 320 nm-340 nm.

The manufacturing process of the standard curve equation comprises the following steps: accurately weighing a proper amount of vitamin E standard substance, dissolving the vitamin E standard substance by absolute ethyl alcohol, fixing the volume, and diluting the vitamin E standard substance into a series of gradient standard working solutions; and injecting the gradient standard working solution into a high performance liquid chromatograph to determine the peak area of the vitamin E, drawing a standard working curve by taking the concentration as an abscissa and the peak area of the vitamin E as an ordinate, and calculating to obtain a standard curve equation.

Compared with the prior art, the invention has the following remarkable effects:

at present, no report of a liquid chromatography detection method related to the vitamin E content in the textile is searched. The method disclosed by the invention is simple to operate, high in sensitivity, good in linear relation within the range of 2.0-100.0 mu g/mL, more than 0.999 of linear correlation coefficient and 0.05mg/kg of detection limit.

Drawings

FIG. 1 is a high performance liquid chromatogram of standard vitamin E;

FIG. 2 is a graph of a standard working curve for vitamin E;

FIG. 3 is a high performance liquid chromatogram of vitamin E in a textile sample.

Detailed Description

The present invention is illustrated below with reference to specific examples, however, the scope of the present invention is not limited to only the following examples. After reading the teaching of the present invention, the skilled in the art can make various changes or modifications to the invention, and these equivalents also fall within the scope of the claims appended to the present application.

Example 1

A determination method for rapidly detecting the content of vitamin E in textiles comprises the following steps:

(2) accurately weighing a proper amount of vitamin E standard substance, ultrasonically dissolving the vitamin E standard substance by absolute ethyl alcohol, fixing the volume in a volumetric flask, and diluting the vitamin E standard substance into a series of gradient standard working solutions of 2.0 mu g/mL, 5.0 mu g/mL, 10.0 mu g/mL, 20.0 mu g/mL, 50.0 mu g/mL and 100.0 mu g/mL;

injecting the gradient standard working solution into a high performance liquid chromatograph, measuring by using a fluorescence detector, drawing a standard working curve by taking the concentration as an abscissa and the chromatographic peak area of vitamin E of a measured object as an ordinate, and making a standard curve equation;

the testing conditions of the high performance liquid chromatograph are as follows: the chromatographic column is Agilent Eclipse XDB C18, 4.6x150mm, 5 μm; column temperature: 20-40 ℃; the mobile phase consists of methanol and water, the volume ratio of the methanol to the water is 98:2, the flow rate of the mobile phase is as follows: 1.0 mL/min; the detector is an FLD fluorescence detector, and the detection conditions are as follows: the excitation wavelength is 295nm, and the emission wavelength is 330 nm;

(2) taking a proper amount of textile samples, cutting the textile samples into fragments with the size of no more than 5mm multiplied by 5mm, and uniformly mixing the fragments to obtain a sample; weighing 0.3g of sample (accurate to 0.0001g) and placing into a triangular flask, accurately adding 10ml of absolute ethanol solution, and performing ultrasonic extraction for 20 min; filtering with microporous membrane with pore diameter of 0.45 μm to obtain filtrate as test solution;

(3) and (3) injecting the liquid to be tested obtained in the step (2) into a high performance liquid chromatograph, determining vitamin E and the peak area thereof, calculating the content of the vitamin E in the liquid to be tested according to a standard curve equation, and calculating the content of the vitamin E in the sample.

According to the method, when the concentration of the gradient standard working solution of the vitamin E is 2.0 mu g/mL, 5.0 mu g/mL, 10.0 mu g/mL, 20.0 mu g/mL, 50.0 mu g/mL and 100.0 mu g/mL, the regression equation y is 2.563x +0.814, and the correlation coefficient R is²When the concentration was 0.999, the detection limit was 0.05 mg/kg.

A positive sample was tested according to the above procedure to obtain a sample with a vitamin E content of 33.82 mg/kg.

Example 2

(1) the standard curve equation and the testing conditions of the high performance liquid chromatograph are the same as those of the embodiment 1;

(2) taking a proper amount of textile samples, cutting the textile samples into fragments with the size of no more than 5mm multiplied by 5mm, and uniformly mixing the fragments to obtain a sample; weighing 0.6g of sample (accurate to 0.0001g) and placing into a triangular flask, accurately adding 20ml of absolute ethanol solution, and performing ultrasonic extraction for 25 min; filtering with 0.45 μm microporous membrane to obtain filtrate as test solution;

(3) and (3) injecting the liquid to be tested obtained in the step (2) into a high performance liquid chromatograph, determining vitamin E and the peak area thereof, and calculating according to a standard curve equation to obtain the content of the vitamin E in the sample to be tested.

A positive sample was tested according to the above procedure to obtain a sample with vitamin E content of 41.52 mg/kg.

Experimental example 1: sample addition recovery rate experiment and precision experiment in example 1

Weighing 0.3g of negative sample, respectively adding low, medium and high 3 concentration levels of vitamin E standard solution, measuring 6 parallel samples at each concentration level, processing according to sample analysis steps, and performing standard recovery rate and precision test, wherein the test results are shown in Table 1.

Table 1 blank recovery of vitamin E in samples (n ═ 6)

The results show that the average recovery rate within 3 addition levels is 99.2-108.9%, and the RSD value is less than 7.90%.

Claims

1. an assay method for rapidly detecting vitamin E content in textiles, is characterized in that, adopt dehydrated alcohol to extract textile sample, extract liquid is filtered, obtain pretreatment test solution; Adopt high performance liquid chromatograph to measure described solution to be tested Vitamin E content in.

2. assay method according to claim 1, is characterized in that, comprises the following steps:

(1) Sample treatment: add anhydrous ethanol to an appropriate amount of sample, ultrasonically extract for 10 to 50 minutes, filter the extract with a microporous membrane with a pore size of 0.20 to 0.45 μm, and use the filtrate as the solution to be tested;

(2) Sample detection: inject the solution to be tested into a high-performance liquid chromatograph to measure vitamin E and its peak area, calculate the content of vitamin E in the solution to be tested according to the standard curve equation, and calculate to obtain the test solution. The content of vitamin E in the samples.

3 . The assay method according to claim 2 , wherein the sample is a textile sample cut into pieces no larger than 5 mm×5 mm. 4 .

4. assay method according to claim 2, is characterized in that, the test condition of described high performance liquid chromatograph is: chromatographic column is Agilent Eclipse XDB C18 or equivalent chromatographic column, 4.6×150 mm, 5 μm; Column temperature: 20～40℃; injection volume: 5～30μL; mobile phase is composed of methanol and water, the volume ratio of methanol and water is (99～90): (1～10), and the flow rate of mobile phase is 0.8～1.5mL/min ; The detector is a FLD fluorescence detector, and its detection conditions are: excitation wavelength 290nm-300nm, emission wavelength 320nm-340nm.

5. assay method according to claim 2, is characterized in that, the preparation process of described standard curve equation is: take by weighing an appropriate amount of vitamin E standard substance accurately, adopt absolute ethanol dissolving back to constant volume, then dilute into a series of gradient standards Working solution; inject the gradient standard working solution into a high performance liquid chromatograph to measure the peak area of vitamin E, take the concentration as the abscissa and the peak area of vitamin E as the ordinate, draw a standard working curve, and calculate the standard curve equation.