Detection method of macrolide antibiotics in honey and its sample processing method

Abstract

The invention discloses a method for detecting macrolide antibiotics in honey and a sample treatment method thereof. The sample treatment method comprises the steps of curing a film-forming dispersionliquid composed of PAN, a DMF solution and ZIF-8@ GO powder on a metal sheet to form a film, thereby obtaining a PAN cross-linked ZIF-8@ GO film coating; diluting the honey sample, extracting, washing and eluting with a PAN cross-linked ZIF-8@ GO film coating, and blow-drying eluent to obtain a treated honey sample. The obtained treated honey sample is directly determined by one or more of theexisting macrolide antibiotic determination methods. The method is simple, convenient and rapid to operate, accurate in detection result and capable of being widely applied and popularized.

Description

technical field [0001] The invention relates to the technical field of antibiotic detection, in particular to a detection method of macrolide antibiotics in honey and a sample processing method thereof. Background technique [0002] Honey is a natural sweet substance that is produced by one or more of the nectar, secretions, honeydew, etc. collected by bees from the flowers of flowering plants through multiple transformations in the bees or fully brewed in the hive. Honey is rich in nutrients and has extremely complex ingredients. It mainly contains natural glucose and fructose, and also contains protein, inorganic salts, organic acids, multivitamins, calcium, magnesium, potassium, phosphorus, etc. It is a popular natural health food . At present, in order to reduce the mortality of bees and increase honey production in bee breeding, a variety of drugs are used, among which quinolones and macrolides are two commonly used antibiotics, and the use of drugs causes more drug re...

AI Technical Summary

Problems solved by technology

[0004] The composition of honey is complex, which greatly interferes with the detection of macrolide antibiotics. The detection error of macrolide antibiotics directly using honey as a sample is large. In the prior art, the honey sample is generally processed before the sample Subsequent instrumental analysis, for example: Chinese patent ZL201010181345.3 discloses a method for simultaneous determination of lincomycin and macrolide residues in royal jelly by liquid chromatography tandem mass spectrometry, including standard solution preparation, royal jelly sample Processing, standard curve making and royal jelly sample detection process; In the royal jelly sample processing process, use acetonitrile ammonia water with a volume concentration of 97% as the extract, including: a, first weigh 5 g of the royal jelly sample and add 10 ml of water to obtain the royal jelly sample liquid; b, Then put the royal jelly sample solution in a 100ml centrifugal plastic bottle, then add 100 μl of roxithromycin internal standard temporary standard solution with a concentration of 200 μg / kg to the 100 ml centrifugal plastic bottle and vortex and mix for 3 minutes, then let it stand for 15 minutes and then pour Add 40ml of acetonitrile ammonia water extract with a volume concentration of 97% to a 100ml centrifugal plastic bottle and mix evenly, then perform ultrasonic extraction on the liquid in the 100ml centrifugal plastic bottle for 10min, and then centrifuge at a speed of 3000rpm for 5min to obtain No. 1 supernatant Liquid; absorb 25ml No. 1 supernatant and put it into 50ml No. 1 centrifuge bottle, then slowly add 10g of anhydrous Na to the 50ml No. 1 centrifuge bottle 2 SO 4 Vigorously vibrate and dehydrate immediately afterwards, then centrifuge at 3000rpm for 2min to obtain the No. 2 supernatant, place the No. 2 supernatant in a 50ml glass centrifuge bottle, and then place 5ml of acetonitrile ammonia water extract with a volume concentration of 97% in 50ml No. 1 centrifuge bottle, then slowly add 10g of anhydrous Na to the 50ml No. 1 centrifuge bottle 2 SO 4 Immediately shake and dehydrate vigorously, then centrifuge at a speed of 3000rpm for 2 minutes to obtain the No. 3 supernatant, and place the No. 3 supernatant in a 50ml glass centrifuge bottle; Concentrate under reduced pressure below 35°C to dryness to obtain the residue, then transfer the residue to a 15ml plastic centrifuge tube with 5ml phosphate buffer solution, then add 5ml ethyl acetate to the 15ml plastic centrifuge tube and mix thoroughly, then extract for 1min, and then The liquid in the 15ml plastic centrifuge tube was centrifuged at 3000rpm for 5min and separated into layers, then the ethyl acetate layer was placed in a 10ml centrifuge tube and dried with nitrogen, and then 1ml of the initial mobile phase was added to the 10ml centrifuge tube and ultrasonically dissolved , then add 2ml of n-hexane and vigorously shake manually to fully mix and remove fat, then centrifuge at 800rpm for 2min to obtain the lower layer sample liquid, pass the lower layer sample liquid through a 0.22μm filter membrane to obtain the test sample liquid on the machine; the sample The treatment method uses an organic solvent (97% acetonitrile and ammonia water) for extraction, and the pretreatment method after extraction includes steps such as dehydration, centrifugation, rotary evaporation, nitrogen blowing, etc., and the process is cumbersome

Chinese patent ZL201110022494.X discloses a liquid chromatography tandem mass spectrometry isotope dilution method for simultaneous determination of multiple types of drug residues in honey. This method directly dilutes the sample with a phosphate buffer solution (pH=8) and then uses HLB solid phase extraction to purify, Determination by liquid chromatography tandem mass spectrometry, quantification by isotope internal standard dilution internal standard method and external standard method; the sample processing specifically includes: weighing 5g sample, accurate to 0.01g, placing it in a 50mL stoppered centrifuge tube, adding 0.1mL Isotope internal standard solution, add 20mL phosphate buffer solution to dilute, mix well, and wait for purification; purification: transfer the diluted honey solution to the HLB solid-phase extraction cartridge, discard the effluent, add 20mL water to rinse, drain, 6mL For eluting with methanol, control the flow rate at 1mL / min-2mL / min, collect the eluate, concentrate under reduced pressure in a water bath below 40°C to nearly dryness, dilute to volume with 2.0mL methanol aqueous solution, mix well, pass the solution through a 0.22μm filter membrane, and supply Determination by liquid chromatography tandem mass spectrometer; this method uses HLB solid phase extraction method for purification and elution, the method is simple and easy to operate, but the number of samples that can be detected at one time is not large, and the whole process of sample processing requires technicians to operate

[0005] At present, the detection method of macrolide antibiotics in honey is widely used as solid-phase extraction method, which uses traditional adsorption material solid-phase extraction column for extraction, which cannot detect a large number of samples, and the efficiency is low

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