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5.
2.
4.
7 Selection of analysis conditions
(1) Selection of solid phase extraction column for purification sample
In the study of this method, Oasis HLB solid phase extraction column, BUND ELUT C 18 solid phase extraction column, ENVI-18 solid phase extraction column, Octadecyl C 18 solid phase extraction column, LiChrolut EN solid phase extraction column and Sep-Pak were used The C 18 solid phase extraction column has a total of six solid phase extraction columns to compare the extraction efficiency and purification effects of six penicillins
.
Experiments have found that the Sep-Pak C18 solid phase extraction column has a low recovery rate (only 50% to 60%) and the purification effect is not ideal.
(2) Selection of extraction solution
Deionized water, 4% sodium chloride solution and 0.
1 mol/L sodium dihydrogen phosphate buffer solution (pH 9.
0) were used as extracting solutions to complete the recovery rate experiment of 6 penicillins in honey samples
.
The experiment found that the recovery rates of the three extracts were in the range of 78.
Table 5-29 The influence of three extracts on recovery rate (%)
(3) Selection of eluent and dosage of OasisHLB solid phase extraction column
This method compares the effects of using acetonitrile and methanol as the eluent of OasisHLB solid phase extraction column on the recovery of six penicillins
.
The experiment found that using acetonitrile as the eluent and the amount within 3 mL, all 6 penicillins could be completely eluted from the OasisHLB column
The elution conditions of 6 penicillins were tested with 0.
5-5 mL methanol respectively, and the results are shown in Table 5-30
.
From Table 5-30, it can be seen that the recovery rate of OasisHLB solid phase extraction column with 3mL methanol eluting 6 kinds of penicillins is above 90%.
Table 5-30 The influence of the amount of eluent of OasisHLB solid phase extraction column on the recovery rate (%)
(4) Selection of liquid chromatography analysis column
The μBondapak C 18 300mm×4.
0mm chromatographic column and the SunFire TM 3.
5um C 18 150mm×2.
1mm chromatographic column were compared respectively
.
Experiments have found that the sensitivity of these two chromatographic columns can meet the requirements, but the μBondapak C 18 300mm×4.
