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Method for detecting cyanolabe in textiles by reversed phase high performance liquid chromatography

A reversed-phase high-performance liquid chromatography and chromatographic detection technology, which is applied in the field of reversed-phase high-performance liquid chromatography to detect blue pigments in textiles, can solve problems such as differences in the applicability of carcinogenic aromatic amines, uncertain conversion rates, and difficult judgments, and achieve linearity The effect of good relationship, ensuring accuracy, and high extraction separation effect

Inactive Publication Date: 2009-03-25
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0006] ② Due to the use of carcinogenic aromatic amines as raw materials, and the conversion rate of most coupling reactions is not quantitative, these carcinogenic aromatic amines are entrained in the final product;
[0038] (3) The conditions of extraction and concentration are different in applicability to carcinogenic aromatic amines, especially aromatic amines that are easily oxidized;
[0040] (5) The precision and repeatability of the method are poor
[0042] 3 Chemical composition and hazards of blue pigment
[0046] And because the azo dye monitoring method is prohibited in German textiles by reducing the azo dye, measure the reduction product to determine the content of the azo dye, use this method to measure the blue pigment, the substance in the solution after extraction is very complicated (see figure 1 ), under the premise of unknown blue pigment structural formula, it is difficult to judge which peaks in the chromatogram are related to blue pigment, and it is impossible to accurately and reliably detect blue pigment and its content in textiles
And at present, our country has not publicly released a feasible method for detecting blue pigment, so that the inspection work of this project cannot be carried out. Therefore, it is urgent to study an accurate, reliable, sensitive inspection method and related technologies to meet the needs of the development of green textiles.

Method used

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  • Method for detecting cyanolabe in textiles by reversed phase high performance liquid chromatography
  • Method for detecting cyanolabe in textiles by reversed phase high performance liquid chromatography
  • Method for detecting cyanolabe in textiles by reversed phase high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] 1 Experimental instruments and reagents

[0079] 1.1 Experimental Instruments

[0080] Shimadzu LC-10AT high performance liquid chromatography, Kromsil ODS-1 C18, 5μ, 250mm×4.6mm chromatographic column; SPD-10A ultraviolet detector, SCL-10A recorder, KQ-500DE numerical control ultrasonic cleaner, electric heating Blast drying oven. FINNIGAN LCQ DECA XP MAX liquid mass spectrometer.

[0081] 1.2 Drugs and reagents

[0082] Acetonitrile Chromatographically pure

[0083] Methanol Chromatographically pure

[0084] Ethanol Chromatographically pure

[0085] Potassium dihydrogen phosphate analytically pure Tianjin Beilian Fine Chemicals Development Co., Ltd.

[0086] Sodium hydroxide Analytical grade Guangzhou Chemical Reagent Factory

[0087] Triethylamine analytically pure

[0088] Phosphoric acid analytically pure

[0089] C 39 h 23 ClCrN 7 o 12S.2Na standard sample (purity 93%).

[0090] 2 sample preparation

[0091] 2.1 Extraction sample preparation:

[00...

Embodiment 2

[0115] The difference from Example 1 is:

[0116] Standard curve: Measure 0.201mg / ml, 0.100mg / ml, 0.080mg / ml, 0.060mg / ml, 0.040mg / ml and 0.020mg / ml standard solutions prepared in 2.2 of Example 1 and inject 20μl each into the liquid chromatograph Instrument, according to the above method configuration standard solution was measured by reversed-phase high-performance liquid chromatography, and the peak area was measured at 254nm wavelength. With the concentration as the abscissa and the peak area as the ordinate, draw a standard curve ( Figure 6 ).

[0117] The resulting regression equation is:

[0118] (2) Y=aX+b, (a=3.703613e-008, b=2.870155e-003), R=0.9996135

[0119] Determination of blue pigment content in the sample to be tested: take the actual sample prepared in 2.1, and carry out high-performance liquid chromatography determination with the chromatographic conditions of 3.1: the peak area is 1405145, select the standard curve (2), and the measured concentration of ...

Embodiment 3

[0121] 1 Experimental instruments and reagents are the same as in Example 1

[0122] 2 Sample preparation

[0123] 2.1 Extraction sample preparation:

[0124] A single dyed textile sample was cut into small pieces of 3.5 cm x 3.5 cm. The weighed weight was 0.5562g. Place the sample in a 50mL colorimetric tube, add 15mL of methanol:water=80:20 mixed solution, place in an ultrasonic bath with a frequency of 450W, and extract at (70±2)°C for 30min. The extract was cooled at room temperature and filtered through a polytetrafluoroethylene membrane filter with a pore size of 0.45 μm. Avoid excessive contact with other plastic polymers when filtering. Pour the extract into a 1mL sample bottle, tighten the Teflon cap, and save it for later use.

[0125] 2.2 Standard sample preparation is the same as in Example 1

[0126] 2.3 Mobile phase equipment:

[0127] Potassium dihydrogen phosphate and potassium phosphate mixed solution: Weigh 2.60 grams of potassium dihydrogen phosphate ...

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Abstract

The invention discloses a method for detecting cyanine in textile through reversed-phase high-efficiency liquid chromatography. The method comprises the following steps: (1) a solution of a sample to be detected is prepared; (2) a standard solution is prepared; (3) the standard solution is taken out, is injected to a high-efficiency liquid chromatographic instrument and is mensurated through a reversed-phase high-efficiency liquid chromatography method; the peak-out position of the cyanine is mensurated by a liquid chromatography-mass spectrometry instrument; the peak-out area is recorded; with concentration as an abscissa and the peak-out area as an ordinate, a standard curve equation is manufactured; and (4) according to the method in step (3), the cyanine and the peak-out area in the solution of the sample to be detected are mensurated; and the obtained standard curve is used to obtain the content of the cyanine in the sample to be detected through calculation. The method can accurately, reliably and sensitively mensurate the cyanine and the content of the cyanine in the textile.

Description

technical field [0001] The invention relates to a method for detecting blue pigment in textiles, in particular to a method for detecting blue pigment in textiles by reverse-phase high performance liquid chromatography. Background technique [0002] At present, about two-thirds of the synthetic dyes in the world market are made on the basis of azo chemistry, that is, about two-thirds of the synthetic dyes are azo dyes, and it is estimated that there are about 2,000 varieties with an annual output of nearly 600,000 tons. According to the application category of dyes, they belong to acid dyes, ice dyes, direct dyes, reactive dyes, disperse dyes, cationic dyes, basic dyes and solvent dyes. [0003] 1 Importance and harm of azo dyes [0004] The two basic reactions in the manufacture of azo dyes are diazotization and coupling. The reaction of aromatic primary amine (also known as diazonium component) and nitrous acid to form diazonium salt is called diazotization reaction. Fact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 邓志光梁勇刘崇华叶湖水张晓利徐敏黄伯熹李慧兰丽丽李光毅
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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