ABSTRACT
Objective:To establish a method for the determination of the potential genotoxic impurities [ methyl chloroacetate and ( R, S) 4-ethyl chloro-3-hydroxybutyrate ] in oxiracetam raw material .Methods:GC-MS was conducted , and the potential genotoxic impurities were extracted by ethyl acetate .The column was a VF-1701 ms capillary column (30 m ×0.25 mm, 0.25 μm) with pro-grammed temperature and the inlet temperature was 220 ℃.The column flow was 1.0 ml· min-1 and the purge flow was 5.0 ml· min-1 .The split injection was used and the split ratio was 5:1 .The carrier gas was high purity helium and the detector was a mass spectrometer detector .The ion source temperature was 230℃and the interface temperature was 230 ℃.The delay time of solvent was 4 min and the ionization mode was electron impact .The scanning ( detection ) method was selective ion monitoring , the electron energy was 70 eV, and the injection volume was 1.0 μl.Results:The separation between the impurities met the requirements .The concen-tration linear range was 50-400 ng· ml-1 (r≥0.9995).The recoveries were 89.7％-96.3％ (RSD=2.3％, n=9) and 91.0％-105.3％(RSD=4.4％, n=9), respectively.Conclusion:The method is simple, accurate, sensitive and rapid, and can be used for the determination of two potential genotoxic impurities in oxiracetam raw material .
ABSTRACT
Objective:To establish a wavelength switching HPLC with gradient elution for the simultaneous determination of six active components, [(R,S)-goitrin, salvianolic acid B, tanshinone IIA, luteolin-7-glucoside, 4-hydroxyacetophenone and scoparone ] in Ganyan Kangfu pills .Methods:An Agilent TC-C18 (250 mm ×4.6 mm, 5 μm) chromatographic column was used with the mobile phase consisting of acetonitrile and 0.1％ phosphoric acid solution with gradient elution .The flow rate was 0.9 ml· min-1 , and the column temperature was 25 ℃.( R,S)-Goitrin was detected at 245 nm, salvianolic acid B and tanshinone IIA were detected at 270 nm, luteolin-7-glucoside was detected at 348 nm, 4-hydroxyacetophenone and scoparone were detected at 278 nm.The sample volume was 10 μl.Results:The linear range of (R,S)-goitrin, salvianolic acid B, tanshinone ⅡA, luteolin-7-glucoside, 4-hydroxyacetophe-none and scoparone was 1.99-49.75 μg· ml-1(r=0.9999), 18.66-466.50 μg· ml-1(r=0.9994), 2.25-56.25 μg· ml-1(r=0.9998), 2.62-65.50 μg· ml-1(r=0.9998), 2.48-62.00 μg· ml-1(r=0.9992) and 2.55-63.75μg· ml-1(r=0.9996), respectively.The average recovery was 98.42％(RSD=0.83％), 99.56％(RSD=1.04％), 97.96％(RSD=1.53％), 96.84％(RSD=0.78％), 98.10％(RSD=1.44％) and 97.82％(RSD=1.34％)(n=6), respectively.Conclusion: The method with good reproducibility is simple and accurate , which provides a new way for the quality evaluation of Ganyan Kangfu pills .
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Objective:To prepare enteric-coated pellets of ( R)-rabeprazole sodium and investigate the drug release behavior in vitro. Methods:The pellets of ( R)-rabeprazole sodium were prepared by a fluid bed coating technology, and HPMC and Eudragit L30D-55 was used as the material of isolation layer and enteric coating, respectively. The similarity of in vitro drug release was com-pared between the reference preparation and the self-prepared preparation. Similar factor ( f2 ) was used to evaluate the similarity of re-lease curves. Results:The coating formula of ( R)-rabeprazole sodium enteric-coated pellets was as follows: the weight of HPMC E5 and Eudragit L30D-55 was 12. 0% and 45. 0%, respectively, and the plasticizer was 8. 0% of the weight of the polymers. The f2 of the reference preparation and the self-prepared preparation was more than 50, which indicated the release behavior was similar. Con-clusion:The release behavior of ( R)-rabeprazole sodium enteric-coated pellets is quite promising, and the preparation technology can be used in the industrial production.
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Objective To establish a HPLC method for simultaneous determination of uracil,hypoxanthine,guanosine, thymine,and( R,S)-goitrin in Isatidis Radix. Methods The determination was performed on a Hanbon Hedera C18 column (4. 6 mm×250 mm,5 μm). The mobile phase consisted of acetonitrile( A)and water( B)with linear gradient elution at the flow rate of 1.0 mL·min-1. The column temperature was 30 ℃. Detection wavelength was 254 nm. Results The linear range of uracil,hypoxanthine,guanosine,thymine,and(R,S)-goitrin was 1.97-39.40 mg·L-1(r=0.999 9),1.25-50.00 mg·L-1(r=0.999 9),0.25-10.40 mg·L-1(r=0. 999 6),2. 84-56. 70 mg·L-1(r=0. 999 9),and 0. 72-28.80 mg·L-1(r=0.999 8), respectively. The average recovery was 99. 36%(RSD=0. 91%),99. 79%(RSD=1. 12%),100. 90%(RSD=1. 71%),98. 67%(RSD=1. 50%),and 99. 33%(RSD=0. 94%),respectively. Conclusion The method is simple,accurate,reliable,reproducible and sensitive,which can be used as an effective method for quality control of Isatidis Radix.