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A kind of detection method of dehydrocholic acid in aquatic product

A detection method and technology of dehydrocholic acid, which are applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as large economy, dyspnea, skin irritation, etc., and achieve the effects of good extraction effect, high sensitivity and high recovery rate.

Active Publication Date: 2022-03-11
厦门泓益检测有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, adding bile acids to feed can promote the healthy cultivation of aquatic products and improve economic benefits, but at the same time, excessive bile acids will accumulate and remain in aquatic products, and human consumption contains bile acids, such as dehydrocholic acid. Aquatic products may have adverse reactions such as belching, hiccups, diarrhea, nausea, muscle spasms, skin irritation around the rectum, etc. If they are consumed for a long time or if they are taken too much at one time, it may lead to electrolyte imbalance, and even dyspnea and heartbeat. Severe reactions such as cardiac arrest, cardiac arrhythmia, muscle spasm, extreme fatigue and weakness
[0003] The Korean Food and Drug Administration has established a residue limit standard for dehydrocholic acid in aquatic products, stipulating that dehydrocholic acid in aquatic products shall not exceed 0.01mg / kg; Among them, from January 2018 to August 2019, a total of 2 batches of aquatic products in China were found to be unqualified for dehydrocholic acid residues, and they were found consecutively in July and August 2019, resulting in a large economic loss
On the contrary, there is no standard method for the detection of dehydrocholic acid in aquatic products in my country, and there are basically no detection methods at home and abroad. Therefore, it is urgent to establish a set of sensitive, accurate and rapid detection methods for dehydrocholic acid residues in aquatic products. Provide technical means for the detection of dehydrocholic acid residues in aquatic products exported to South Korea

Method used

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  • A kind of detection method of dehydrocholic acid in aquatic product
  • A kind of detection method of dehydrocholic acid in aquatic product
  • A kind of detection method of dehydrocholic acid in aquatic product

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Experimental program
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Embodiment approach

[0032] 1. Instruments, reagents and materials

[0033] Dehydrocholic acid standard (purity 99.04%, Stanford Analytical Chemicals Inc.);

[0034] β-glucuronidase / arylsulfatase (Shanghai Anpu Experiment Technology Co., Ltd.);

[0035] Ammonium acetate (≥98.0%, Xilong Science Co., Ltd.);

[0036] Acetic acid (≥99.8%, Sinopharm Chemical Reagent Co., Ltd.);

[0037] Ammonium acetate buffer solution (weigh 15.4g ammonium acetate, dilute to 1L with ultrapure water, adjust pH to 5.2 with appropriate amount of acetic acid);

[0038] Ethyl acetate, methanol, acetonitrile (chromatographically pure, German Sigma company);

[0039] IKA MS3Digital vortex mixer digital display type, constant temperature oscillator (Changzhou Guohua Electric Co., Ltd.);

[0040] Nitrogen blowing instrument (Shanghai Anpu Experimental Technology Co., Ltd.);

[0041] Ruisijie Unique+UV laboratory multifunctional pure water-ultrapure water system (Xiamen Ruisijie Scientific Instrument Co., Ltd.);

[0042] ...

Embodiment

[0062] Three commercially available aquatic products, yellow croaker meat, prawn meat and oyster meat, were used as test objects, respectively spiked with 2 μg / kg and 10 μg / kg, and parallel experiments were performed at the same time (n=6). The recovery rate and RSD were determined in Table 2 . The results showed that the recoveries of dehydrocholic acid ranged from 80.15% to 103.33% under the conditions of two spiked concentrations, and the relative standard deviation RSD (n=6) ranged from 2.93% to 5.42%. The test results meet the requirements for exporting Korean aquatic products.

[0063] Table 2 Standard recovery rate

[0064]

[0065] Using this detection method, two domestic batches of aquatic products were detected by South Korea as unqualified samples of dehydrocholic acid residues, and the detected content of dehydrocholic acid was 0.001-0.004 mg / kg. The results are shown in Table 3.

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Abstract

The present invention relates to a method for detecting additives in aquatic products, in particular to a method for detecting dehydrocholic acid in aquatic products, preparing a standard solution, soaking samples of aquatic products in ammonium acetate buffer saline solution, and adding β-glucuronidase / Arylsulfatase enzymatic hydrolysis overnight, ethyl acetate extracted the target substance, concentrated to dryness by nitrogen blowing, then constant volume with methanol, detected by liquid chromatography-triple quadrupole mass spectrometry, and quantified by external standard method, the obtained standard The correlation coefficient R of the curve 2 >0.999, dehydrocholic acid has a good linear relationship in the concentration range of 1, 2, 5, 10 and 50ng / mL, and the detection limit of dehydrocholic acid is 0.117μg / kg. This method is fast, simple, sensitive Accurate, environmentally friendly and cheap, it has practical application and guiding significance for the detection of dehydrocholic acid residues in aquatic products. The recovery rate, repeatability, sensitivity and detection limit all meet the detection limit requirements for aquatic products exported to South Korea.

Description

technical field [0001] The invention relates to a method for detecting additives in aquatic products, in particular to a method for detecting dehydrocholic acid in aquatic products. Background technique [0002] Dehydrocholic acid is a kind of bile acid. Bile acid is a series of sterol substances produced in the process of cholesterol metabolism in animals. Because it is mainly excreted into the intestinal tract through the gallbladder and bile, and is acidic, it is collectively called bile. acid. The types and amounts of bile acids vary from animal to animal. Bile acid has surface activity because its molecular structure is amphoteric, with an alkyl group at one end, which is lipophilic and can be combined with oils and fats, and a hydroxyl and carboxyl group at the other end, which is hydrophilic. Therefore, the most important function of bile acids in animals is to digest fat and fat-soluble substances (fat-soluble vitamins and cholesterol, etc.) in food. Secondly, bil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 邹明宇付加亮郭亚圈
Owner 厦门泓益检测有限公司