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5.
2.
1.
7 Selection of analysis conditions
(1) Selection of solid phase extraction column
In the study of this method, OasisHLB solid phase extraction column, BUNDELUT C 18 solid phase extraction column, ENVI-18 solid phase extraction column, Octadecyl C 18 solid phase extraction column, LiChrolutEN solid phase extraction column and Sep-Pak C 18 solid phase extraction column were used.
A total of six solid phase extraction columns were used to compare the extraction efficiency and purification effects of nine penicillins
.
The experiment found that the recovery rate of Sep-Pak C 18 solid phase extraction column is low (only 50% to 60%), and the purification effect is not ideal.
(2) Selection of extraction solution
Deionized water, 4% sodium chloride solution and sodium dihydrogen phosphate buffer solution (0.
15 mol/L, pH 8.
5) were used as extraction solutions to complete the recovery rate experiment of 9 penicillins in the sample
.
Experiments have found that when deionized water and 4% sodium chloride solution are used as the extract, the recovery rates of amoxicillin and ampicillin are both less than 30%, and the other seven penicillins are in the range of 78.
Because the concentration and pH of the sodium dihydrogen phosphate buffer solution have a greater impact on the recovery rates of amoxicillin and ampicillin, the buffer solutions of sodium dihydrogen phosphate with different concentrations of 0.
033~0.
2mol/L and the pH of 0.
15mol/L are respectively prepared at 3.
0~0.
2mol/L.
9.
5 Sodium dihydrogen phosphate buffer solution, complete the recovery rate experiment of amoxicillin and ampicillin, the results are shown in Table 5-8
.
Experiments show that when the concentration of sodium dihydrogen phosphate is 0.
Table 5-7 The influence of three extracts on the recovery rate of 9 penicillins
Table 5-8 The influence of different concentration and pH of sodium dihydrogen phosphate buffer solution on the recovery rate of amoxicillin and ampicillin
(3) Selection of elution conditions for solid phase extraction column
This method compares the effect of using 1mL, 2mL, 3mL, 4mL acetonitrile -water (1+1, v/v) as the eluent of the solid phase extraction column on the recovery rate of 9 penicillins.
The results are shown in Table 5-9.
Table 5-9 The effect of solid phase extraction column eluent dosage on recovery rate (%)