HPEC For The Determination Of Anthraquinones And Sulfonamides,Fluoroquinolones Residues

Chapter one: The capillary electrophoresis and accelerated solvent extraction technique were described simply. The analytical research and development status of anthraquinones,sulfonamides and fluoroquinolones were reviewed.Chapter two: A novel nonaqueous capillary electrophoresis(NACE) method with diode-array detection was developed for effective separation and simultaneous determination of the three anthraquinones. A BGE solution of 40 m M Na Ac-40 m M NH4Ac-40 m M Na OH in methanol was used for separation of the three anthraquinones. Under the optimized conditions,the analytes can be effectively separated in 7 min. The standard curves of the three anthraquinones showed good linearity, with correlation coe fficients of r > 0.999. The limit of detection of aurantio-obtusin, emodin and rhein was 0.25, 0.12 and 0.19 mg/ml, respectively.Their average intra- and inter-day analytical precisions(relative standard deviation) were less than 2.8% and 4.0%, respectively. The recoveries of the three spiked levels of aurantio-obtusin, emodin and rhein from semen cassiae and cassia seed tea samples were in the range of 86.6–106%. The proposed method provides the speediness, selectivity, sensitivity,linearity and accuracy as well as low reagent consumption necessary for simultaneous analysis of the test anthraquinones. The ultrasonic extraction–NACE method could be applied for quality control of semen cassiae and cassia seed tea.Chapter three: A rapid analytical method is developed for effective separation and rapid simultaneous determination of six anthraquinones(aurantio-obtusin, aloe-emodin, rhein,emodin, chrysophanol, and physcion) by capillary zone electrophoresis(CZE). A rapid and effective sample preparation procedure without clean up step using accelerated solvent extraction(ASE) with acetonitrile as solvent.was presented. Under the optimized CZE conditions, the effective separation of six anthraquinones was achieved within runtime of 8min. Good linearity was achieved, with a correlation coefficient(r) of ≥0.999. The limit of detection was in the range of 0.33–1.40 μg/m L. The intra-day RSD(n=6) of the six analytes was in the range of 2.3–3.9%, and inter-day RSD(n=9) was in the range of 3.2–4.9%. The average recovery of the six analytes from real tea samples was in the range from 86.15 to98.30% with the RSD of 1.04–4.99%. The developed and validated method has speediness,high sensitivity, recovery and precision, and can be applied for the quality control of semen cassiae and cassiae seed teaChapter four: A novel method for simultaneous determination of sulfonamides(Sulfadiazine, sulfametoxydiazine, Sulfadimethoxypyrimidine) and fluoroquinolones(Lomefloxacin, enoxacin, sarafloxacin, enrofloxacin) by large volume sample stacking-capillary zone electrophoresis( LVSS-CZE) has been proposed. The determination conditions containing p H,concentration of Na2B4O7 and methanol, separation voltage, injection time were optimized.The operating buffer was composed of 25 m M Na2B4O7(20%methanol, p H=8.8) with a constant temperature of 20℃. The separation voltage was 25 k V and injection time was 60 s. Good linearity was achieved, with a correlation coefficient(r) of ≥0.999, The detection limit of lomefloxacin, enoxacin, sarafloxacin,enrofloxacin, sulfadiazine, sulfametoxydiazine, sulfadimethoxypyrimidine was 0.025, 0.033,0.025, 0.020, 0.013, 0.013, and 0.013 μg/ml, respectively. The recoveries were 90.5%, 91.3%,90.6%, 90.5%, 89.9%, 88.8%, and 88.1%, respectively.