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Method for determining alkyl quaternaries cation surface active agent by liquid phase chromatography -tandem mass spectrometry combined technology

A technology of surfactant and alkyl quaternary ammonium, which is applied in the detection field of alkyl quaternary ammonium salt cationic surfactant, can solve problems such as poor qualitative effect, and achieve the effect of high selectivity, accurate analysis method and accurate qualitative

Inactive Publication Date: 2008-11-26
CENT TESTING INT GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Method used

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  • Method for determining alkyl quaternaries cation surface active agent by liquid phase chromatography -tandem mass spectrometry combined technology
  • Method for determining alkyl quaternaries cation surface active agent by liquid phase chromatography -tandem mass spectrometry combined technology
  • Method for determining alkyl quaternaries cation surface active agent by liquid phase chromatography -tandem mass spectrometry combined technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Using isopropanol as solvent, a series of standard solutions of dioctadecyldimethylammonium chloride were prepared according to Table 1, and analyzed and detected by liquid chromatography-tandem mass spectrometry technology LC / MS / MS according to the above experimental conditions. figure 1 It is the chromatogram of detected dioctadecyldimethylammonium chloride, the ordinate in the chromatogram represents the intensity of the peak, and the abscissa represents the retention time. Depend on figure 1 It can be seen that the target substance elutes quickly, and the retention time is 4.32min. Concentration is plotted with peak area, according to 3 parallel measurement results of standard solution, establishes the standard curve of dioctadecyl dimethyl ammonium chloride, as figure 2 As shown, the ordinate in the standard curve represents the response value of the liquid chromatography peak area, and the abscissa represents the concentration of dioctadecyldimethylammonium chlo...

Embodiment 2

[0026] Accurately weigh 1 gram of the fabric treatment agent sample into a conical flask, add an appropriate amount of isopropanol to the round bottom flask, place it in an ultrasonic wave, and conduct ultrasonic extraction at room temperature for 2 hours. Extract in this way three times, combine the extracts, filter, dilute the mother liquor in a 10 ml volumetric flask with isopropanol, and take the mother liquor for liquid chromatography-tandem 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 2, and the first parallel sample (test number A) was repeatedly measured 6 times, and the analysis results were shown in Table 3. Known from Table 2, the relative standard deviation (RSD) of parallel samples is 2.73%. Known from Table 3, the relative standard deviation of repeated tests is 0.21%.

[0027] The test content of dioctadecyl dimethyl ammonium chloride in this ...

Embodiment 3

[0032] The standard solution in Example 1 was added to the fabric treatment agent 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 80% and 105%.

[0033] Table 3 The recovery of standard addition of this sample

[0034]

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Abstract

The invention relates to a method for detecting the cationic surfactants of alkyl quaternary ammonium salts with the liquid chromatography-tandem mass spectrometry and includes the following steps: pre-treating the detected samples with a Soxhlet extraction method or a supersonic extraction method; detecting with a liquid chromatograph-tandem mass spectrometer with the LC conditions of a C18 reverse-phase chromatographic column, a column temperature of 30 to 60 DEG C, the inlet volume of 3 to 10ul, the mobile phase flow rate of 0.15 to 0.60ml per minute; the tandem mass spectrometry MS / MS is provided with the conditions of ionizing by adopting the electro-spray ionization model and the detection mode of multi-ion reaction. The method adopted by the invention is characterized by accurate and fast analysis method, high method selectivity, little interference, etc.

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 liquid chromatography-tandem mass spectrometry. 【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 Cation...

Claims

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Application Information

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IPC IPC(8): G01N30/00G01N30/89
Inventor 杨果王鑫刘蔷薇何树悠梁圆圆郭冰
Owner CENT TESTING INT GRP CO LTD
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