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Method for detecting residual amount of streptomycin and dihydrostreptomycin in tomato sauce

A technique for dihydrostreptomycin and ketchup, which is applied to measuring devices, instruments, scientific instruments, etc., can solve the problems of poor peak shape, low sensitivity, and great influence on the measurement of the analyte, and achieves less reagent consumption and higher sensitivity. High, precise effects

Inactive Publication Date: 2014-04-09
新疆出入境检验检疫局检验检疫技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above substances have a great influence on the determination of streptomycin and dihydrostreptomycin by liquid chromatography mass spectrometry. When the purification conditions are not good, the peak shape of the analyte is very poor and the sensitivity is very low

Method used

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  • Method for detecting residual amount of streptomycin and dihydrostreptomycin in tomato sauce
  • Method for detecting residual amount of streptomycin and dihydrostreptomycin in tomato sauce
  • Method for detecting residual amount of streptomycin and dihydrostreptomycin in tomato sauce

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Effect test

Embodiment 1

[0031] Weigh the tomato paste sample in a centrifuge tube, add the extract to the sample, vortex, oscillate, ultrasonicate, and centrifuge, take 7.0 ml of the above centrifuged supernatant in a 15 ml centrifuge tube, and pour it into the centrifuge tube at the same time Add 0.8 g of diatomaceous earth, vortex, oscillate, and centrifuge, take 4.0ml of the centrifuged supernatant and use a double-column series of hydrophilic-lipophilic equilibrium solid-phase extraction column and weak cation-exchange solid-phase extraction column to simultaneously Purification; series hydrophilic-lipophilic equilibrium solid-phase extraction column is column 1; weak cation exchange solid-phase extraction column is column 2; use 5.0 ml methanol and 5.0 ml water to respectively activate hydrophilic-lipophilic equilibrium solid-phase extraction column and weak For cation-exchange solid-phase extraction cartridges, wash column 1 and column 2 with 6.0 ml of phosphate buffer solution, add 6.0 ml of wa...

Embodiment 2

[0034] The present invention considers that the content of lycopene in the tomato sauce is relatively high, and also contains various minerals, carbohydrates, carotene, vitamins, proteins, fats, riboflavin, niacin and folic acid and other substances. The ingredients in tomato sauce are very complex and varied.

[0035] The above-mentioned impurities have a great influence on the determination of streptomycin and dihydrostreptomycin by liquid chromatography tandem mass spectrometry. When the purification conditions are not good, the interference of the matrix is ​​very serious, the peak shape of the analyte is very poor and the sensitivity is very low. Purification treatment is a difficult problem in the determination of streptomycin and dihydrostreptomycin.

[0036] The initial purification of dispersive solid-phase extraction mainly uses some adsorbents, such as polyamide, alumina, florisil, diatomaceous earth and activated carbon, to remove polar or non-polar interference su...

Embodiment 3

[0038] The purpose of re-purification is to remove some polar substances and pigments and acids that were not removed by the initial purification. The present invention mainly utilizes a solid phase extraction column (SPE). Generally, there are two ways to use the SPE column. One is to use the SPE column to retain the analyte; the other is to use the SPE column to retain some impurities. In the prior art, a reversed-phase column and an ion-exchange column are used to purify twice respectively. This operation requires ion-pair reagents, and the consumption of elution reagents is large, and the operation is cumbersome and time-consuming. The present invention utilizes a hydrophilic-lipophilic equilibrium column (upper part: column 1) and an ion exchange column (lower part: column 2) to be connected in series to simultaneously purify samples. First of all, the present invention takes into account the strong polarity of the analyte, and when no ion-pairing reagent is used, there i...

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Abstract

The invention discloses a method for detecting the residual amount of streptomycin and dihydrostreptomycin in tomato sauce. The method comprises the following steps of: weighing a sample of the tomato sauce and putting the sample in a centrifuge tube; adding an extracting solution; performing whirling, shaking, ultrasonic treatment and centrifugation; fetching 7.0ml of supernate and putting in the centrifuge tube, and adding 0.8g of kieselguhr; performing whirling, shaking and centrifugation; fetching 4.0ml of supernate and purifying at the same time by use of a hydrophilic and lipophilic equilibrium solid-phase extraction column and a weak cation exchange solid-phase extraction column which are connected in series; activating the two columns by use of 5.0ml of methanol and 5.0ml of water respectively; loading the sample; leaching the two columns by use of 6.0ml of extracting solution, 6.0ml of water and 1.0ml of methanol in turn; eluting by use of 6.0ml of methanol containing 3% formic acid; blowing to dryness by use of nitrogen; and dissolving the residue by use of 0.5ml of acetonitrile containing 0.2% formic acid and an formic acid for the LC-MS / MS (liquid chromatogram-tandem mass spectrometry) measurement. The method disclosed by the invention has the characteristics of fastness in detection, sensitivity, accuracy and economical efficiency, wide practicability and the like.

Description

field of invention [0001] The invention belongs to the field of food safety detection. Specifically, the invention relates to the technical field of detection of streptomycin and dihydrostreptomycin residues in tomato paste. Background technique [0002] Streptomycin (Streptomycin) and Dihydrostreptomycin (Dihydrostreptomycin) are commonly used drugs in aminoglycoside antibiotics. Inhibit peptide chain extension and bacterial protein synthesis, eliminate Gram-negative aerobic bacteria and some Gram-positive bacteria. It has a good control effect on a variety of plant bacterial and fungal diseases, especially bacterial diseases, such as tomato bacterial wilt, tomato canker, Chinese cabbage soft rot and cucumber bacterial angular spot, etc. . However, this antibiotic has certain toxic and side effects on people. If excessive streptomycin remains in the food, it will cause serious harm to the human body, such as damage to the vestibular nerve and cochlear nerve leading to hea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/14
Inventor 巩志国季新成李世雨员丽娟苏敏尚德军
Owner 新疆出入境检验检疫局检验检疫技术中心
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