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1 Scope of application
Royal jelly and lyophilized powder suitable for the metronidazole , Dimetridazole , tinidazole , Ronidazole , Turney metronidazole, isopropyl metronidazole , metronidazole and hydroxylation, hydroxylation isopropyl metronidazole, Determination of 9 nitroimidazoles residues in 2-hydroxymethyl-1-methylated-5-nitroimidazole by liquid chromatography-tandem mass spectrometry
.
Detection limit of royal jelly: 0.
5μg/kg, detection limit of lyophilized powder: 1.
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3.
2 Principle of the method
Royal jelly and lyophilized powder contains metronidazole, dimenidazole, tinidazole, lonidazole, tenidazole, isopropnidazole, as well as hydroxylated metronidazole, hydroxylated isoprenidazole, 2- Hydroxymethyl-1-methylated-5-nitroimidazole 9 kinds of nitroimidazole drug residues, dissolved in sodium acetate buffer, liquid-liquid extraction with ethyl acetate, after rotary evaporation to dryness, add carbon tetrachloride And acid-containing aqueous solution, centrifuged to take the upper solution, liquid chromatography-tandem mass spectrometry determination
.
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3 Reagents and materials
Acetonitrile, methanol, ethyl acetate , formic acid: chromatographically pure; carbon tetrachloride, sodium acetate: analytically pure metronidazole, dimenidazole, tinidazole, lonidazole, tenidazole, and isoprenidazole , And hydroxylated metronidazole, hydroxylated isopronidazole, 2-hydroxymethyl-1-methylated-5-nitroimidazole standard substance purity ≥98%
.
The internal standard is deuterated 2-hydroxymethyl-1-methylated-5-nitroimidazole (HMMNI-D 3 ; CAS: 8061-52-7), deuterated hydroxylated isopropnidazole (IPZ-OH- D 3 ; CAS: 8061-52-7); the purity of deuterated substances is ≥95%
.
Standard stock solution: 1000μg/mL
.
Accurately weigh 10.
0mg±0.
Sodium acetate buffer solution: 0.
1mol/L.
Accurately weigh 8.
Aqueous formic acid: 0.
1%
.
Accurately pipet 1 mL of formic acid, dilute to a 1000 mL volumetric flask with water, mix with ultrasound and degas for 15 minutes, and place it in a liquid chromatography mobile phase flask for use
.
Matrix mixed standard working solution: According to the sensitivity of the standard material and the linear range of the instrument, draw a certain amount of the intermediate concentration mixed standard solution, and use the blank sample extract to prepare a series of concentrated matrix mixed standard working solution
.
Temporary use and provisioning
.
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4 Instruments and equipment
Liquid chromatography-tandem rod mass spectrometer: equipped with atmospheric pressure chemical ionization source (or equivalent ionization source); high performance liquid chromatography equipped with online degasser, low residue autosampler, temperature-controlled column oven and High-precision mixing pump; electronic analytical balance: sensitivity 0.
1mg and 10mg; refrigerated centrifuge: speeds up to 4000r/min and 13000r/min; nitrogen blowing instrument: water bath and heating temperature control; desktop disperser; rotary concentrator: with Vacuum evaporation and circulating cooling water; ultrapure water device; ultrasonic cleaner; multifunctional food grinder; vortex mixer; chicken heart flask: 125mL; centrifuge tube: 15mL and 50mL; PTFE material; volumetric flask: 10mL and 1000mL
.
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5 Sample pretreatment
(1) Sample preparation
Mix liquid, slurry, and powder samples thoroughly; pulverize and grind solid samples stored at low temperature for testing
.
When necessary, the laboratory samples are divided into quarters
.
(2) Extraction
Weigh about 2.
5~5.
0g sample (Royal jelly weighs 5.
0g±0.
2g; lyophilized powder weighs 2.
5g±0.
2g) into a 50 mL centrifuge tube, and add the deuterated marker HMMNI-D.
IPZ-OH respectively -D 3 100 μL, add 20 mL of sodium acetate solution and fully vortex and shake for 1 min
.
Then add 20 mL of ethyl acetate, after vortexing and liquid-liquid extraction, transfer all the ethyl acetate layer into the chicken heart steaming flask, repeat the above operation, combine the three ethyl acetate extracts in the chicken heart steaming flask, and concentrate below 40℃ Nearly dry, remove the solvent
.
(3) Purification
The residue of the chicken heart steaming flask was dissolved with 1 mL carbon tetrachloride and 1 mL formic acid aqueous solution, and vortexed thoroughly for 1 min
.
Aspirate the upper aqueous solution and filter with a microporous filter membrane (0.
2 μm).
This is the test solution
.
Related links: Linear range and lower limit of determination of metronidazole, ronidazole and dimetridazole residues in honey