CN104049046A - Method for detecting dimethyl fumarate in body lotion - Google Patents

Abstract

The invention belongs to the technical field of body lotion detection and in particular relates to a method for detecting dimethyl fumarate in body lotion. The method comprises the following steps: taking a body lotion sample to be detected, and adding the sample into cyclohexanone ethyl acetate according to a mass volume ratio of 1:4, wherein a volume ratio of cyclohexanone to ethyl acetate is 1:1; shaking and performing ultrasonic treatment for 15 minutes, and filtering through a filter membrane of 0.5 micron; separating by adopting GPC, wherein the impurity discard time is 400 seconds, and the collection time is 401-600 seconds; and performing gas chromatography-mass spectrometer (GC-MS) analysis on the solution obtained in the step 3. The method is simple, feasible and high in operability; conventional reagents are adopted, and compared with actual operation, the method has the advantages that the cyclohexanone and ethyl acetate are added, the sample solution is good in effect during GPC separation, the measurement indexes such as accuracy, precision and sensitivity can achieve good effects, and an effective way is provided for standard detection.

Description

Dimethyl fumarate detection method in a kind of milky lotion

Technical field

This patent belongs to the dimethyl fumarate detection method in a kind of milky lotion detection technique field, especially milky lotion.

Background technology

Dimethyl fumarate is referred to as DMF.It has the feature of low toxicity, efficient, broad-spectrum antiseptic, and mould is had to special fungistatic effect.Can be applicable to the mildew-resistant of bread, feed, fish, meat, vegetables, fruit, textiles and leathers goods.DMF is better than calcium propionate greatly for the anti-mold effect of bread.Show according to domestic research, DMF has good fungal resistance, be better than the acid antiseptics such as propionate, sorbic acid and benzoic acid for the anti-mold effect of feed, containing many moulds and bacterium being played to complete inhibiting effect in the PDA nutrient culture media of 500～800 ppm, can make that food is difficult for going mouldy, long shelf-life, can also keep bright in colour.

But excessive contact dimethyl fumarate can damage enteron aisle, internal organ and cause allergy, can change in vivo methyl alcohol, eyes are stared to organ detrimental effect, if children's contact more can be grown and cause very large harm it.

GPC(Gel Permeation Chromatography), gel permeation chromatography, be called again size exclusion chromatography (Size Exclusion Chromatography, be called for short SEC), it is the separating mechanism based on volume exclusion, by thering is the fixing phase of molecular sieve character, be used for separating the material that relative molecular mass is less, and can analyzing molecules volume difference, there is the macromolecule homolog of identical chemical property.But in milky lotion, more due to adjuvant, essence and flavoring agent, complicated component, therefore, if carry out suitable processing, makes testing result accurately and reliably, become the current problem that solves of needing.

Summary of the invention

The present invention aims to provide the dimethyl fumarate detection method in a kind of effective, reliable milky lotion.

Dimethyl fumarate detection method in milky lotion of the present invention, comprises the steps:

Step 1, get milky lotion sample to be detected, join in cyclohexanone ethyl acetate according to mass volume ratio 1:4, wherein the volume ratio of cyclohexanone and ethyl acetate is 1:1;

Step 2, jolting, after ultrasonic 15 minutes, through 0.5 μ m membrane filtration;

Step 3, employing GPC separate, and it is 400s that impurity abandons the time; Acquisition time is 401s ~ 600s;

Step 4, the solution that step 3 is obtained carry out GC-MS analysis.

Method of the present invention is simple, all adopt conventional reagent, workable, contrast through practical operation, discovery adds cyclohexanone and ethyl acetate, sample solution is effective in the time that GPC separates, and the indexs such as the accuracy of measurement, precision, sensitivity all can reach better effects, for the effective approach that provides is provided in standardization.

Brief description of the drawings

Fig. 1 is embodiment sample total ion current figure.

Fig. 2 is embodiment sample mass spectrogram.

Embodiment

Dimethyl fumarate detection method in milky lotion of the present invention, comprises the steps:

Step 1, get milky lotion sample to be detected, join in cyclohexanone ethyl acetate according to mass volume ratio 1:4, wherein the volume ratio of cyclohexanone and ethyl acetate is 1:1.

Step 2, jolting, after ultrasonic 15 minutes, through 0.5 μ m membrane filtration.

Step 3, employing GPC separate, in the present embodiment, what GPC gel permeation chromatograph was selected is German LC-TECH product, the design parameter that GPC separates is: filler is selected the Bio-Beads S-X3 gel filler (purchasing from upper Haiquan island scientific & trading Co., Ltd. Room 1701, No. 1 building, Shanghai, address business section Yang Lu Lane 455) of 30.0g; Sample size is 5ml; Mobile phase is cyclohexanone and ethyl acetate (volume ratio is 1:1), and it is 400s that impurity abandons the time; Acquisition time is 401s ~ 600s; It is 400s that impurity abandons the time; Acquisition time is 401s ~ 600s; Every 50s collects a duplicate samples, high-order vacuum laser degree 180mbar; Low level vacuum laser degree 210mbar; Thickening temperature is 50 DEG C, and concentrated rear constant volume is 2ml.

Step 4, the solution that step 3 is obtained carry out GC-MS analysis.GC-MS coupling condition, chromatographic column is selected: 5% phenyl methyl polysiloxane capillary column, 30m*0.32mm, 0.25 μ m; Initial 60 DEG C of column temperature, is warming up to 280 DEG C with 20 DEG C/min speed, keeps 2min; Carrier gas in post (high-pure helium) flow 1.0ml/min, injection port is not shunted; Solvent delay time 4min, 250 DEG C of temperature; 230 DEG C of detecting device ion source temperatures; 250 DEG C of interface temperature; 250 DEG C of level Four bar temperature; EMv1076; Ion scan scope 50 ~ 400 μ, sample size 1 μ L; Select ion monitoring pattern, quantitatively selecting ion is 113,85,59.In accompanying drawing, Fig. 1 is embodiment sample total ion current figure, and Fig. 2 is embodiment sample mass spectrogram.

Claims (1)

1. the dimethyl fumarate detection method in milky lotion, is characterized in that comprising the steps:

Step 1, get milky lotion sample to be detected, join in cyclohexanone ethyl acetate according to mass volume ratio 1:4, wherein the volume ratio of cyclohexanone and ethyl acetate is 1:1;

Step 2, jolting, after ultrasonic 15 minutes, through 0.5 μ m membrane filtration;

Step 3, employing GPC separate, and it is 400s that impurity abandons the time; Acquisition time is 401s ~ 600s;

Step 4, the solution that step 3 is obtained carry out GC-MS analysis.