CN104062386A - Pretreatment method for determining content of formaldehyde in marine products - Google Patents

Abstract

The invention belongs to the technical field of food detection, and particularly relates to a pretreatment method for determining the content of formaldehyde in marine products. The method is simple and easy, adopts the conventional reagent and is strong in operability. Discovered from comparison of actual operation, due to addition of potassium ferrocyanide and zinc acetate, the separating effect of a sample solution is good, a better effect can be achieved for the indexes such as the accuracy, the precision and the sensitivity of measurement, and an effective path is provided for standard detection.

Description

A kind of preprocess method of measuring content of formaldehyde in marine product

Technical field

This patent belongs to a kind of food inspection technical field, especially measures the preprocess method of content of formaldehyde in marine product.

Background technology

Formaldehyde is a kind of colourless, gas of having intense stimulus smell.Soluble in water, alcohol and ether.Formaldehyde is gaseous state at normal temperatures, conventionally occurs with aqueous solution form.Formaldehyde mainly contains the following aspects to health hazard:

A, spread effect: the main harm of formaldehyde shows as the spread effect to skin and mucosa, formaldehyde is protoplasmic poison material, can while suction, occur that stimulation and oedema, eye that respiratory tract is serious stimulate, headache with protein bound, high concentration.

B, sensitization: the direct Formaldehyde Exposed of skin can cause allergic dermatitis, color spot, necrosis, can bring out bronchial astehma while sucking high-concentration formaldehyde.

C, mutagenesis: high-concentration formaldehyde or a kind of genotoxicity material.Animal used as test, in the situation that laboratory high concentration sucks, can cause rhinopharyngeal neoplasm.

D, outstanding behaviours: headache, dizzy, weak, nauseating, vomiting, uncomfortable in chest, ophthalmodynia, have a throat-ache, that stomach is received is poor, palpitaition, have a sleepless night, lose weight, failure of memory and vegetative nervous disorder etc.; The long-term suction of pregnant woman may cause fetal anomaly, and even dead, the long-term suction of man can cause man's teratospermia, death etc.

China's food additives use in hygienic standard and clearly specify to forbid to add formaldehyde and compound thereof, therefore need the objective food kind to adding formaldehyde to monitor.

Formaldehyde Jia Ce main method has spectrophotometric method, vapor-phase chromatography, high performance liquid chromatography etc. at present, if carry out suitable pre-service for detected sample, makes testing result more accurate, becomes problem to be solved.

Summary of the invention

The present invention aims to provide the preprocess method of content of formaldehyde in a kind of mensuration marine product of simple and fast.

In mensuration marine product in the present invention, the preprocess method of content of formaldehyde, comprises the steps:

Step 1, get marine product sample 10g to be detected, add after 5ml potassium ferrocyanide and 5ml zinc acetate, be settled to 100ml.

After step 2, vibration evenly, leave standstill and be no less than 30 minutes, filter.

Step 3, preparation DNPH acetonitrile solution, DNPH is 3:5 with the quality g of acetonitrile and the ratio of volume L.

Step 4, get 5ml filtrate, add DNPH acetonitrile solution 10ml, deionized water 10ml, mix.

Under step 5,40 DEG C of conditions, after ultrasonic extraction 40min, take out and be cooled to room temperature.

Centrifugal 2 minutes of step 6,10000r/min, get supernatant and cross 0.45 μ m filtering with microporous membrane, is disposed, for liquid chromatogram measuring.

Method of the present invention is simple, all adopt conventional reagent, workable, contrast through practical operation, discovery adds potassium ferrocyanide and zinc acetate, sample solution good separating effect, 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 marine product sample chromatogram figure to be measured.

Embodiment

Below in conjunction with specific embodiment, the preprocess method of content of formaldehyde in the mensuration marine product in the present invention is described as follows.

Step 1, get marine product sample 10g to be detected, add after 5ml potassium ferrocyanide and 5ml zinc acetate, be settled to 100ml;

After step 2, vibration evenly, leave standstill and be no less than 30 minutes, filter;

Step 3, preparation DNPH acetonitrile solution, DNPH is 3:5 with the quality g of acetonitrile and the ratio of volume L;

Step 4, get 5ml filtrate, add DNPH acetonitrile solution 10ml, deionized water 10ml, mix;

Under step 5,40 DEG C of conditions, after ultrasonic extraction 40min, take out and be cooled to room temperature;

Centrifugal 2 minutes of step 6,10000r/min, get supernatant and cross 0.45 μ m filtering with microporous membrane, is disposed, for liquid chromatogram measuring.

Measuring chromatographic condition is as follows: select C ₁₈chromatographic column (4.6mm*250mm, m), mobile phase is selected the methanol-water solution that volume ratio is 7:3 to 5 μ, and flow velocity 1ml/min, detects wavelength 365nm; 30 DEG C of column temperatures, sample size 10 μ L.Upper machine testing, obtains in accompanying drawing, and Fig. 1 is marine product sample chromatogram figure to be measured.

Claims (1)

1. measure a preprocess method for content of formaldehyde in marine product, it is characterized in that comprising the steps:

Step 1, get marine product sample 10g to be detected, add after 5ml potassium ferrocyanide and 5ml zinc acetate, be settled to 100ml;

After step 2, vibration evenly, leave standstill and be no less than 30 minutes, filter;

Step 3, preparation DNPH acetonitrile solution, DNPH is 3:5 with the quality g of acetonitrile and the ratio of volume L;

Step 4, get 5ml filtrate, add DNPH acetonitrile solution 10ml, deionized water 10ml, mix;

Under step 5,40 DEG C of conditions, after ultrasonic extraction 40min, take out and be cooled to room temperature;

Centrifugal 2 minutes of step 6,10000r/min, get supernatant and cross 0.45 μ m filtering with microporous membrane, is disposed, for liquid chromatogram measuring.