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Method for testing alkyl quaternaries cationic surfactant

A surfactant and alkyl quaternary ammonium technology, which is applied in the detection field of alkyl quaternary ammonium cationic surfactants, can solve the problems of expensive detection instruments and poor qualitative results, and achieve cheap instruments and accurate analysis methods , the effect of little interference

Inactive Publication Date: 2008-09-03
CENT TESTING INT GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, by adding organic reagents such as dibromocarboxyphenyldiazoaminoazobenzene, an association color reaction occurs with alkyl quaternary ammonium salt surfactants in alkaline medium, and then analysis by spectrophotometry is also a kind of Methods for the detection of cationic surfactants based on alkyl quaternary ammonium salts; however, these methods have the disadvantage of poor qualitative results when interfering substances are present
Studies have shown that the use of atmospheric pressure electrospray mass spectrometry (ESI / MS) connected to high-performance liquid chromatography for analysis, the qualitative analysis of its structure and composition according to the molecular weight information provided by mass spectrometry, and the quantitative analysis of high-performance liquid chromatography can be accurately qualitative and quantitative. Two or more mixed surfactants in daily chemical cleaning products, this method has little interference, but the detection equipment used is expensive

Method used

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  • Method for testing alkyl quaternaries cationic surfactant
  • Method for testing alkyl quaternaries cationic surfactant
  • Method for testing alkyl quaternaries cationic surfactant

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Using isopropanol as a solvent, a series of standard solutions of dioctadecyldimethylammonium chloride were prepared, and the gas chromatography-mass spectrometry GC-MS analysis and detection were carried out according to the above experimental conditions. The sample port temperature was set at 300°C; the interface temperature was set at 250°C; the carrier gas was helium, and the flow rate was 1 ml / min; Raise the temperature to 210°C and keep it for 2 minutes, then raise the temperature to 320°C at a speed of 20°C / min and keep it for 2 minutes; The source temperature was 250 °C; the injection volume was 1 microliter. Figure 1a It is the chromatogram of the detected dioctadecyldimethylammonium chloride decomposition product, the ordinate in the chromatogram represents the intensity of the peak, and the abscissa represents the retention time; Figure 1b It is the mass spectrogram of the detected dioctadecyldimethylammonium chloride decomposition product chlorooctadecane,...

Embodiment 2

[0030] Accurately weigh 0.5 g of the hair conditioner sample into a conical flask, add an appropriate amount of isopropanol into the round bottom flask, place it in an ultrasonic field, and conduct ultrasonic extraction at room temperature for 2 hours. Extract in this way three times, combine the extracts into a round-bottomed flask, concentrate the extracts by rotary evaporation, dilute to a 50 ml volumetric flask with isopropanol, take 10 ml, dry with anhydrous sodium sulfate, filter, and take the mother liquor for gas chromatography - Mass spectrometry test. Three parallel samples were made to this sample, the test numbers were A, B and C respectively, and the analysis results were shown in Table 1, and the first parallel sample (test number A) was measured 5 times, and the analysis results were shown in Table 2. Known from Table 1, the relative standard deviation (RSD) of parallel samples is 3.29%. Known from Table 2, the relative standard deviation of repeated tests is 0...

Embodiment 3

[0036] The standard solution in Example 1 was added to the hair conditioner sample in Example 2, and the experiment was carried out according to the above-mentioned sample pretreatment method and instrumental analysis and detection method. Four spiked levels were made to the sample, and the average value was obtained by three parallel measurements for each sample with the spiked content. According to the actual amount added and the measured results, the spiked recovery rate of the sample was calculated. The experimental results are shown in Table 3. It can be seen from Table 3 that the recovery rate of the samples was between 95% and 105%.

[0037] Table 3 The recovery of standard addition of this sample

[0038]

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Abstract

The invention provides a method for testing the alkyl quaternary ammonium salt cationic, which includes the following steps: processing a pretreatment for the test sample; testing with a gas-chromatography-mass spectrometer, setting the injection port temperature of the instrument at 180-350 EDG C, setting the carrier gas flow rate at 0.5-2.0 ml per minute, the chromatographic column is a nonpolar, weak polar or strong polar column, setting the port temperature at 180-300 EDG C; injecting the pretreatmented sample into the chromatographic column through the injection port of the instrument, processing the programmed temperature, from 40-120 EDG C up to 210-320 EDG C, processing the mass spectrometric detection after each component of the decomposition products of the sample is separated by the chromatographic column. The method provided by the invention has the merits of cheap test instrument, safety, accurate and fast analysis method and small disturbance, which causes the alkyl quaternary ammonium salt cationic in the sample to pyrolyze on the injection port, and processes the optimized separation of each component of the pyrolyzed products.

Description

【Technical field】 [0001] The invention relates to a detection method for alkyl quaternary ammonium salt cationic surfactants, in particular to a method for detecting alkyl quaternary ammonium salt cationic surfactants by means of gas chromatography-mass spectrometry technology. 【Background technique】 [0002] Cationic surfactants have been widely used as fungicides, fabric softeners, antistatic agents, hair conditioners, etc., and are one of the important chemical raw materials in the washing industry and cosmetics industry. Alkyl quaternary ammonium salts with hydrophobic groups directly attached to nitrogen atoms are the simplest and most widely used cationic surfactants. Because alkyl quaternary ammonium salt cationic surfactants can provide excellent static control ability, wet combing and dry combing properties, deep conditioning effect and good additive properties, they are often used in hair conditioner formulations; in addition, alkyl quaternary ammonium salts Catio...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/54G01N30/06
Inventor 杨果王鑫何树悠刘蔷薇梁圆圆郭冰
Owner CENT TESTING INT GRP CO LTD
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