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A kind of detection method of olaquindox in the premix containing organic chromium

A detection method and premix technology, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve problems such as weak absorption strength, low response, and interference with olaquindox, so as to reduce interference, improve accuracy, and improve extraction effects Effect

Active Publication Date: 2020-06-16
正大康地农牧集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it was found in daily testing work that when organic chromium such as chromium picolinate and biological chromium was added to the feed, because the retention time of organic chromium and olaquindox was very similar, the chromatographic peaks almost overlapped, and the resolution was less than 0.1, which seriously interfered with the olaquindox. If the peak shape cannot accurately detect the content of olaquindox, it will seriously interfere with the accuracy of olaquindox detection and affect the determination of the test results.
The results of ultraviolet-visible spectral scanning (190-600nm) show that olaquindox, chromium picolinate, and biochromium all have strong absorption peaks near 260nm, but only olaquindox has absorption peaks near 382nm. Chromium picolinate and biochromium are here There is no ultraviolet absorption signal peak at the place. If other conditions remain unchanged, directly adjust the detection wavelength from 260nm to 382nm. The absorption intensity of the organic chromium-containing premix at 382nm is weak, the response is low, and the detection sensitivity is not high. The detection results and There is still some deviation in the actual content of olaquindox

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A detection method containing olaquindox in the premix of organic chromium, it may further comprise the steps:

[0034] (1) Pretreatment of samples

[0035] Get the premix 5g (containing chromium picolinate 100mg / kg) that olaquindox content is 8mg / kg, add the NaHCO that concentration is 5% successively 3 5 mL of aqueous solution and 45 mL of 65% methanol aqueous solution were ultrasonically treated at 40° C. for 35 min, and the sample extract was obtained after centrifugation.

[0036] (1-1) Drawing of standard curve

[0037] Prepare standard working solutions of olaquindox at the following concentrations: 0.05 μg / mL, 0.1 μg / mL, 0.5 μg / mL, 1 μg / mL, 5.0 μg / mL, and 10 μg / mL; inject 20 μL of the standard working solutions into samples for high-efficiency liquid Phase analysis, then take the peak area as the ordinate and the content of olaquindox as the abscissa to draw a standard curve.

[0038] (2) Sample measurement

[0039] The sample extract is also purified as fol...

Embodiment 2

[0112] A detection method containing olaquindox in the premix of organic chromium, it may further comprise the steps:

[0113] (1) Pretreatment of samples

[0114] Get the premix 5g (containing chromium picolinate 100mg / kg) that olaquindox content is 8mg / kg, add the NaHCO that concentration is 8% successively 3 5 mL of aqueous solution and 45 mL of 80% methanol aqueous solution were ultrasonically treated at 40° C. for 35 min, and the sample extract was obtained after centrifugation.

[0115] (1-1) Prepare standard working solutions of olaquindox at the following concentrations: 0.05 μg / mL, 0.1 μg / mL, 0.5 μg / mL, 1 μg / mL, 5.0 μg / mL, 10 μg / mL; standard curve line.

[0116] (2) The sample extract adopts the following conditions to carry out HPLC analysis

[0117] The sample extract is also purified as follows before adopting high performance liquid phase detection:

[0118] Add the extract to the activated SPE cartridge, then rinse the cartridge with 0.02mol / L HCl solution, t...

Embodiment 3

[0131] A detection method containing olaquindox in the premix of organic chromium, it may further comprise the steps:

[0132] (1) Pretreatment of samples

[0133] Get the premix 5g (containing chromium picolinate 100mg / kg) that olaquindox content is 8mg / kg, add the NaHCO that concentration is 5% successively 3 5 mL of aqueous solution and 45 mL of 65% methanol aqueous solution were ultrasonically treated at 40° C. for 35 min, and the sample extract was obtained after centrifugation.

[0134] (1-1) Drawing of standard curve

[0135] Prepare standard working solutions of olaquindox at the following concentrations: 0.05 μg / mL, 0.1 μg / mL, 0.5 μg / mL, 1 μg / mL, 5.0 μg / mL, and 10 μg / mL; inject 20 μL of the standard working solutions into samples for HPLC Analysis, then take the peak area as the ordinate, and take the content of olaquindox as the abscissa to draw a standard curve.

[0136] (2) Sample measurement

[0137] Described sample extract adopts following conditions to carr...

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Abstract

The invention belongs to the technical field of the olaquindox detection method, and specifically relates to a detection method of olaquindox in premix containing organic chromium. The detection method of the olaquindox in the premix containing organic chromium is characterized by comprising the following steps: (1)pre-treating the sample, successively adding a weak alkali solution and a methanolaqueous solution in the premix containing the organic chromium, ultrasonically treating and centrifugally separating to obtain a sample extracting solution, wherein the weak alkali solution is sodiumcarbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate aqueous solution; and (2) performing high-performance chromatographic analysis on the sample extracting solution by taking 382nm as the detection wavelength. Through the detection method of olaquindox in premix containing organic chromium disclosed by the invention, the interference of the chromium ion can be reduced, andthe 382nm is used as the detection wavelength, the detection sensitivity is improved, and the detection result accuracy is improved.

Description

technical field [0001] The invention belongs to the technical field of detection methods of olaquindox, and in particular relates to a detection method of olaquindox in a premix containing organic chromium. Background technique [0002] Organic chromium is a common feed additive. Yeast chromium, chromium picolinate and chromium nicotinate are common forms of organic chromium. Trivalent chromium can increase the activity of insulin and participate in the synthesis of protein and the metabolism of nucleic acid and fat. It can reduce the fat content in the body, promote the rapid growth of livestock and poultry by reducing blood sugar and fat, and improve the return rate of feed, so it can be added to the feed according to the limit requirements. [0003] Lalaquindox, also known as quinamide alcohol, is widely used in livestock and poultry feed for antibacterial and growth-promoting effects. However, due to its moderate to obvious cumulative toxicity, olaquindox has obvious ter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/36
CPCG01N30/02G01N30/06G01N30/36G01N2030/062
Inventor 陆学文范彪陈华栋
Owner 正大康地农牧集团有限公司