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6.
1.
4.
1 Pre-processing method
(1) Extraction
1) Macrolides
MALs are weakly alkaline, slightly soluble in water, and easily decomposed in aqueous solutions, especially in acidic conditions
.
Commonly used extraction reagents include methanol , acetonitrile , ether , and mixed solvents and buffer solutions such as metaphosphoric acid -methanol, Tris buffer solution, MCI-Vain-EDTA buffer solution, and borate buffer solution
Zhao Donghao et al.
used acetonitrile to extract MALs from pork, then defatted with n-hexane , cleaned up with C 18 column, and eluted with 4% ammoniated methanol.
Liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used in multiple reaction monitoring ( MRM) mode for quantitative and qualitative analysis
.
The limit of detection (LOD) for tilmicosin and kitasamycin is 0.
Horie et al.
extracted with 0.
3% metaphosphoric acid～methanol (7+3, v/v), and simultaneously detected 5 MALs in meat by high performance liquid chromatography (HPLC)
.
The recovery rate at the level of 1.
Dubois et al.
extracted five MALs from meat, kidney, liver, eggs, and milk with tris buffer of pH 10.
5, precipitated proteins with sodium tungstate , purified with solid phase extraction column, and finally analyzed by LC-MS/MS
.
When the concentration of 0.
2) Lincosamides
The commonly used extraction solvents for Lincosamide drugs are generally carbonate buffer and acetonitrile
.
Xu Jinzhong and others established a method for the detection of lincomycin and clindamycin residues in honey
.
The sample was extracted with 0.
3) Macrolides and Lincosamides
Cross-category drug residue analysis, especially in the extraction process, needs to consider the physical and chemical properties of the drug, and try to choose a solvent with strong applicability
.
In the simultaneous analysis of MALs and Lincosamide drug residues, the most commonly used solvent is acetonitrile, and when necessary, auxiliary methods such as pressurized solvent extraction (PLE) can be used to improve the extraction efficiency
Sun Lei and others established lincomycin, clindamycin, pyrithromycin, erythromycin, tylosin, spiramycin, tilmicosin, elixomycin, and kititamycin in animal-source foods.
, Clarithromycin, azithromycin, roxithromycin and josamycin and other 13 kinds of lincosamide and MALs residue detection ultra performance liquid chromatography (UPLC)-MS/MS method
.
The tissue samples were extracted with acetonitrile, dehydrated with anhydrous sodium sulfate, centrifuged, the supernatant was collected, and the fat and other impurities were removed with n-hexane, and then detected by UPLC-MSMS
Related Links: Allowable maximum residues of macrolides and lincosamide drugs
