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6.
2.
2.
7 Selection of analysis conditions
(1) Selection of extraction solution
The main extraction solutions for extracting macrolides from samples are 0.
1mol/L phosphate buffer solution, 0.
1mol/L sodium bicarbonate buffer solution, and 0.
1molL Tris buffer solution.
Comparative experiments have been carried out on this, and the experimental results are shown in Table 6-17
.
Table 6-17 Extraction effect of different extraction solutions (%)
As can be seen from the data in Table 6-17, when using a phosphate buffer solution as the extracting solution, erythromycin , spiramycin , josamycin , oleandomycin recovery less than 80%; when using bicarbonate When sodium solution is used as extracting solution, the recovery rate of spiramycin is less than 70%; and the range of recovery rate is relatively large (68.
3%~139%); when Tris buffer solution is used as extracting solution, the recovery rate is 83.
5%~115.
0 % Range, and the recovery rate is relatively stable
.
Therefore, this method uses 0.
(2) The effect of buffer solutions of different pH on the recovery rate (%)
In the selection experiment of the optimal pH range of 0.
1mol/L Tris buffer solution, it was found that when the pH changes in the range of 5 to 11, the antibiotic recovery rates of lincomycin, echinomycin, and kitasamycin are relatively relatively High and stable
.
The recovery rates of erythromycin, spiramycin, tilmicosin, josamycin, and tylosin vary greatly, from 42.
Table 6-18 The effect of buffer solutions with different pH on recovery rate (%)
(3) The influence of different solid phase extraction columns on the recovery rate
Under the aforementioned selected conditions, the extraction efficiency of three solid phase extraction columns, Oasis MCX (150 mg), Oasis HLB (200 mg) and Oasis HLB (500 mg), were compared
.
In terms of performance, there is no difference between Oasis HLB (200mg) and Oasis HLB (500mg), but due to the different particle size of the two solid phase extraction columns, the particle size of Oasis HLB (200mg) is 30um, and the particle size of Oasis HLB (500mg) is 60um.
Table 6-19 The influence of different solid phase extraction columns on the recovery rate (%)