Determination of p-toluenesulfonylation products of α-cyclodextrin by high-performance liquid chromatography
mono-p-toluenesulf onyl-α-cyclodextrin ester(mono-OTs-α-CD)is an important intermediate for the preparation of other mono-derivatives of α-CD.In this paper,a new liquid chromatography method for the determination of toluenesulfonylation products of α-cyclodextrin was established.Mono-OTs-α-CD on three different carbon sites(C3,C2 and C6)was completely sep-arated on ODS column,and the retention time was 7.70,10.08 and 12.18 min,respectively.The linear regression equations were y=89.176x-559.19(R2=0.999 0),y=87.917x-430.16(R2=0.999 6),and y=70.529x-24.259(R2=0.999 2)over con-centration range from 5 to 500 mg L-1,respectively.The recovery was 92.5～102.3％with RSDs(＜1.8％),and the LOD was less than 0.5 mg L-1,which indicated that high accuracy and precision of this method could meet the monitoring requirements of the above products.The effects of raw material ratio,temperature,time and pH value of the reaction system on the mono-sub-stitution reaction were preliminarily investigated.The optimized conditions(molar ratio of 1∶2,reaction temperature of 15 ℃,reaction time of 15 min)were obtained with a yield of 34.84％(n=3)for mono-3-OTs-α-CD.
high-performance liquid chromatographythe p-toluenesulfonylation products of α-cyclodextrinqualitative and quantitative analysisregionalized derivation
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维普
