Efficient capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in sample
A technology of capillary electrophoresis and sample detection, which is applied in the field of chemical detection to achieve high sensitivity, time saving, good separation and reproducibility
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Embodiment 1
[0057] 1、 Establishment of comparative electrophoresis spectra of standard substances of 11 prohibited compounds such as furazolidone
[0058] (1) Firstly prepare 1 mg / mL standard stock solutions of 11 prohibited compounds for use;
[0059] (2) Take 150 μL of AOZ, AMOZ, SEM, and AHD stock solutions, 150 μL of 50 mmol / L 2-NBA, 0.9 mL of 12 mol / L hydrochloric acid, and dilute to 10 mL with ultrapure water, and derivatize at 70 °C for 1 h;
[0060] (3) Adjust the pH of the derivative solution to 7.4 with 5 mol / L sodium hydroxide;
[0061] (4) Add 300 μL each of furazolidone, furaltadone, nitrofurazone, nitrofurantoin, nifursol, chloramphenicol and ciprofloxacin stock solutions;
[0062] (5) Inject samples under the above electrophoresis conditions to obtain the control electrophoresis spectra of 11 kinds of prohibited compounds such as furazolidone (see figure 1 ).
[0063] 2. Detection limits and concentrations of 11 prohibited compounds including furazolidone (Table 1)
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Embodiment 2
[0074] Yellow bone fish sample detection:
[0075] (1) Preparation of homogeneous extract of yellow-bone fish: Weigh 100 g of homogeneous aquatic product (yellow-bone fish), put it in a 250 mL beaker, extract it ultrasonically with 150 mL of absolute ethanol for 30 min, and then add 80 mL of anhydrous Ethanol, repeated extraction 3 times, combined extracts, centrifuged at 3000 r / min for 10 min, poured the supernatant extract into a round-bottomed flask, concentrated under reduced pressure at 50 °C to nearly dryness, dissolved in 30 mL of acetonitrile and transferred to Add 10 mL of n-hexane to the separatory funnel, extract and separate, discard the n-hexane layer, repeat 5 times, pour the acetonitrile layer into a round-bottomed flask, concentrate under reduced pressure at 50 °C to nearly dryness, dissolve and transfer with absolute ethanol Put it into a graduated test tube, dry it with nitrogen at 50°C, dissolve it with acetonitrile-water (30:70) and dilute to 1 mL.
[0076...
Embodiment 3
[0079] Shrimp sample testing:
[0080] (1) Preparation of shrimp extract: 100 g of homogeneous aquatic product (shrimp) was weighed, placed in a 250 mL beaker, 150 mL of absolute ethanol was ultrasonically extracted for 30 min, 80 mL of absolute ethanol was added again, and the extraction was repeated 3 times. Combine the extracts, centrifuge at 3000 r / min for 10 min, pour the supernatant extract into a round-bottomed flask, concentrate under reduced pressure at 50 °C to nearly dryness, dissolve with 30 mL of acetonitrile and transfer to a separatory funnel, add 10 mL of n-hexane, extracted and separated, discarded the n-hexane layer, repeated 5 times, poured the acetonitrile layer into a round bottom flask, concentrated under reduced pressure at 50 ℃ to near dryness, dissolved with absolute ethanol and transferred to a graduated test tube, at 50 ℃ Blow dry under nitrogen gas, dissolve with acetonitrile-water (30:70) and dilute to 1 mL.
[0081] (2) Shrimp blank sample detect...
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