Preparation method of quality control sample of nitrofuran metabolite residues in fish muscle
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A technology for nitrofuran and quality control samples, which can be used in measuring devices, instruments, scientific instruments, etc., and can solve the problems of long cycle and expensive quality control samples.
Pending Publication Date: 2018-11-16
CHINESE ACAD OF FISHERY SCI
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In the world, only FAPAS provides quality control samples of nitrofuran metabolism in the field of aquatic products, but the quality control samples provided by this institution are expensive and have a long cycle
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[0046] The preparation method of the residual quality control sample of nitrofuran metabolites in the fish muscle of the present embodiment can comprise the following steps:
[0047] Step S1, selection of experimental animals: select negative live fish that meet the preset size and have not been fed with nitrofuran drugs; optionally, the weight of the negative sample of live fish with the preset size is 900g-1100g / strip.
[0048] Step S2, calculating the initial dipping concentration of each nitrofuran drug, and controlling dipping conditions: after the negative sample adapts to the environment, it is dipped for 10 hours under the set conditions, wherein the dipping pool water body It contains four kinds of nitrofuran drugs: furazolidone, furaltadone, nitrofurazone and nitrofurantoin. Each nitrofuran corresponds to an initial dipping concentration.
[0049] Optionally, calculate the initial bath concentration of each nitrofuran original drug according to the linear equation ...
Embodiment 4
[0141] Valuation and Uncertainty Assessment
[0142] The low-concentration lyophilized powder was detected by liquid chromatography-tandem mass spectrometry by 9 accredited laboratories, and the value was determined collaboratively. The results of the value determination and data processing are shown in Tables 14-17.
[0143] Table 14 SEM measurement results of freeze-dried powder in each laboratory
[0144]
[0145] Table 15 AOZ determination results of freeze-dried powder in each laboratory
[0146]
[0147] Table 16 Determination results of AMOZ of freeze-dried powder in each laboratory
[0148]
[0149] Table 17 AHD measurement results of freeze-dried powder in each laboratory
[0150]
[0151] Firstly, the normality of the distribution of all measured data is examined, and the test results by the Shapiro-Wilk method are as follows:
[0152] (1) SEM Shapiro-Wilk method normal distribution test results for freeze-dried powder samples:
[0153] Table 18 SEM d...
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Abstract
The invention discloses a preparation method of a quality control sample of nitrofuran metabolite residues in fish muscle. The preparation method comprises the following steps: selecting negative living fish which meets pre-set specification and size and is not fed by a nitrofuran medicine; carrying out medicine bath treatment under pre-set conditions, wherein a water body of a medicine bath tankcontains four types of nitrofuran drugs including a furazolidone crude drug, a furaltadone crude drug, a furacilin crude drug and a furantoin crude drug; fishing out a positive sample subjected to themedicine bath treatment and killing the fish and taking back muscle to obtain a fish muscle sample; adding a vitamin C solution and uniformly stirring to obtain minced fish; after pre-cooling the minced fish, putting into a freezing drying machine and carrying out freezing drying to obtain a freeze-dried sample; carrying out crushing, blending and sieving treatment on the freeze-dried sample to obtain the quality control sample containing nitrofuran metabolite residues with a target content level. By adopting the scheme, the quality control sample contains four types of nitrofuran metabolitesand can meet the requirements of actual inspection better.
Description
technical field [0001] The invention relates to the technical field of food safety detection, in particular to a method for preparing a quality control sample of residual nitrofuran metabolites in fish muscle. Background technique [0002] Quality control samples are a batch of samples that have sufficient uniformity or multiple chemical, physical, biological, engineering or sensory performance characteristics, have been technically identified, and are accompanied by relevant certificates. In the field of food safety testing, quality control samples play a vital role in ensuring the reliability and accuracy of test results. Foreign residue analysis laboratories have generally used quality control samples for laboratory quality control and judgment of relevant test results on a regular basis. Provided by institutions such as FAPAS, the sample matrix includes urine, animal tissue, etc., and related samples have been industrialized. Domestic residue analysis laboratories ofte...
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