Studies On Analysis Method For Sucralose Synthesis Intermediates

Sucralose(1,6-dichloro-1,6-dideoxy-beta-D-fructofuranosyl-4-chloro-4-deoxy-alpha -D-galactopyranoside)is a high-intensity sweetener derived from sucrose and it is regarded as the highest accomplishment of intense sweetener.Due to its high sweetness,obvious sweetener characteristics and safety,sucralose is used in the manufacturing of artificially sweetened food and drug products.In this paper, sucralose was synthesized using path-of-hologroup-protected as well as methods for the analysis of sucralose and its intermediates were developed.6,1',6'-Tri-O-tritylsucrose-penta-acetate(TRISPA)was analysed by RP-HPLC. The column was Waters XTerra^TMRP₁₈5μm,3.9×150mm;The mobile phase was acetonitrile:water(84:16);The flow rate was 0.6 mL/min;TRISPA was determined with UV detector at 234 nm.Good linearities were obtained within the range from 0.05 to 0.8 mg/mL and the minimum limit of detection was 5 ng(S/N=3).The average recovery of samples were 99.2%and the relative standard derivation was 0.34%.(2)4-PAS and 6-PAS were converted into their trimethylsilyl(TMS)ethers,then identified and quantified by GC-MS and GC respectively,using myo-inositol ester as the internal standard.Good linearities of their TMS ethers were obtained within the range from 0.05 to 0.8 mg/mL of the 4-PAS TMS ether and the minimum limit of detection was 0.25 ng(S/N=3).Precision expressed by the relative standard deviation (RSD)was 0.526%.The average recovery of the method was 98.1%.The 6-PAS TMS ether has a good separation from 4-PAS TMS ether and the conversion process of 4-PAS to 6-PAS was monitored.(3)TOSPA was analysed using RP-HPLC.The column was Waters XTerra^TM RP₁₈5μm,3.9×150 mm;The mobile phase was acetonitrile:water(50:50);The flow rate was 0.6 mL/min;TOSPA was determined with UV detector at 229 nm.Promising linearities were obtained within the range from 0.0125 to 0.1000 mg and the minimum limit of detection was 10 ng(S/N=3).The average recovery of samples were 97.2% and the relative standard derivation was 1.15%.(4)Sucralose was converted into its trimethylsilyl(TMS)ether,then qualified and quantified by GC-MS,GC respectively,using myo-inositol ester as the internal standard.Good linearities of its TMS ethers were obtained within the range from 0.005 to 0.06 mg/mL of the Sucralose TMS ether and the minimum of detection was 0.25 ng(S/N=3).Precision in terms of RSD was 0.626%and the average recovery was 97.95%.