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Objective:To establish a method for the determination of benzene, chlorine alcohol and pyridine residues in piperazine ferulate. Methods:GC was used with a DB-624 (30 m × 0. 53 mm, 1. 0 μm) elastic quartz capillary column. The flame ionization detector was used with nitrogen as the carrier gas. The initial temperature was 50℃, maintaining for 5 min, and raised to 80℃ at the rate of 10℃·min-1 , and then raised to 200℃ at the rate of 50℃·min-1 , and maintaining for 4 minutes. The inlet temperature was 200℃, and the detector temperature was 220℃. The split ratio was 1 ∶1 and the injection volume was 1μl. The flow rate was 3 ml· min-1. Results:The linear range of benzene was 0.16-0.96 μg·ml-1(r=0.999 5), the average recovery was 95.7% (RSD =2.1, n=9), and the detection limit was 0.16 ng. The linear range of chlorine alcohol was 16.11-96.65 μg·ml-1(r=0.999 7), the average recovery was 97. 8% (RSD=2. 1, n=9), and the detection limit was 0. 62 ng. The linear range of pyridine was 15. 87-95. 23 μg·ml-1(r=0. 999 8), the average recovery was 99. 2% (RSD=1. 3, n=9), and the detection limit was 0. 15 ng. Con-clusion:The method is reliable, simple, accurate and stable, and suitable for the determination of benzene, chlorine alcohol and pyri-dine residues in piperazine ferulate.
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Objective:To establish a method for the determination of 7 residual organic solvents including acetone,2,3 -dimethyl-pentane,3-methylhexane,n-heptane,2,2-dimethylhexane,o-xylene and 2,4,6-trimethylpyridine in Shengxuening tablets. Methods: A headspace gas chromatography method was adopted. The determination was performed on a DB-5MS capillary column ( 30 m × 0. 25 mm,0. 25 μm) with programming temperature. Nitrogen was used as the carrier gas at the flow rate of 2. 5 ml·min-1 . The tem-perature of injector was 200℃,and a flame ionization detector was used as the temperature of 250℃. The containers of headspace in-jector were in equilibrium at 95℃ for 30min. DMF was used as the solvent and an external standard method was used for the determi-nation of the 7 residual solvents. The injection volume was 1 ml. Results:Under the chromatographic conditions, the 7 residual organic solvents could be well separated from each other . The concentration of each solvent showed a good linearity with the peak area within the investigated concentration range (r≥0. 994 4). The average recoveries were 98. 72%-99. 71% (RSD=0. 14%-0. 71%)(n=9). Conclusion:The established method is simple, rapid and sensitive, which can be used for the determination of multiple residual or-ganic solvents in Shengxuening tablets.
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Objective:To establish a method for the determination of solvent residues in faeces bombycis extract by GC .Meth-ods: A GC-headspace injection method was adopted to detect the residual organic solvents in the extract of faeces bombycis .A DB-5MS (30 m ×0.25 mm ×0.25 μm) quartz capillary column was used as the chromatographic column;nitrogen was used as the carrier gas at a flow rate of 0.6 ml· min-1;the injector temperature was 200℃;the detector was a flame ionization detector( FID) with the temperature of 250℃;the temperature program included two phases:the initial temperature was set at 40℃for 10 min, and then risen to 200℃at a rate of 5℃· min-1 and maintained for 5 min;the equilibrium temperature of headspace was 95℃;the equilibrium time was 30 min;the capillary temperature was 110℃;the injection ring temperature was 125℃.Results:The linear range of acetone , 2, 3-dimethylpentane, 3-methylhexane, heptane, 2,2-dimethylhexane, p-xylene, m-xylene, O-xylene and 2,4,6-collidine was 101-3 034μg· ml-1 , 100-2 995 μg· ml-1 , 107-3 197 μg· ml-1 , 101-3 019 μg· ml-1 , 99-2 962 μg· ml-1 , 45-1 358 μg· ml-1 , 44-1 325μg· ml-1, 47-1 411 μg· ml-1 and 104-3 130 μg· ml-1, respectively, and the average r was all above 0.992.The recovery of the method met the requirement , and the blank solvent showed no interference .Eight samples were all accordance with the requirements after the examination .Conclusion:The headspace injection method for the determination of residual organic solvents in the extract of faeces bombycis is simple and reliable .
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Objective To establish a headspace GC method for determination of residual organic solvents as methanol, ethanol,dichloromethane and n-hexane in trepibutone. Methods An external standard method was used. A DB-624 capillary column (75 m× 0.450 mm,2.55 μm) was used with a FID detector. The injector temperature was 200 ℃ and the detector temperature was 250 ℃ .The initial column temperature was 50 ℃ ,kept for 6 min,then raised to 200 ℃ at a rate of 20 ℃ ?min-1 and kept for another 12 min. Nitrogen was used as the carrier gas. The flow rate was 3. 0 mL ? min-1 . The headspace vials equilibrium temperature was 80 ℃ and the balance time was 30 min.The injection volume is 1 mL. Results A1l the solvents could be completely separated with good linear relationships.The average recoveries of the four solvents were 100.4% ( RSD =0.5%), 100.6%(RSD = 0.6%), 99.6% ( RSD = 0.8%), 98.7% ( RSD = 0.7%) ( n = 9),respectively. Conclusion The method is simple and accurate,and can be used in the determination of residual solvents in trepibutone.
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Objective:To establish a method for the determination of 8 residual organic solvents in tolterodine tartrate by capillary GC. Methods: The determination of methanol, ethanol, acetonitrile, acetone, ethyl acetate, trichloromethane and tetrahydrofuran in tolterodine tartrate dissolved in the solution of N, N-dimethylformamide-water ( 1∶ 4 ) was carried out on a CP-sil 5CB ( 60. 0 m × 0. 32 mm,5μm)column. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The flow rate of carrier gas was 1. 2 ml·min-1 . The column temperature was 120℃. The headspace vial temperature was 85℃ and the time was 30min. The determina-tion of pyridine in tolterodine tartrate dissolved in the solution of dimethylsulfoxide-sodium hydroxide (17∶13) was carried out on an HP-1(30. 0 m × 0. 53 mm,5 μm) column. The inlet temperature was 220℃ and the FID detector temperature was 250℃. The column tem-perature was 80℃. The flow rate of carrier gas was 3. 0 ml·min-1 . The headspace vial temperature was 85℃ and the time was 30 min. Results:All peaks could be separated from each other under the chromatographic conditions. The linearity of the eight solvents was falrly good (r>0. 999). The average recovery was ranged from 86. 0% to 100. 2% with RSD of 1. 7%-3. 5% (n=9). The limit of detection was 0. 63, 0. 43, 0. 30, 0. 18, 0. 079, 0. 36, 0. 18 and 0. 89 μg·ml-1 , respectively. Conclusion:The methods can be applied in the determination of the eight residual organic solvents in tolterodine tartrate.
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Objective:To establish a method for the determination of dichloromethane, methanol and ethanol in fenticonazole ni-trate. Methods:The samples were detected by headspace GC. The column was OV-1301(30 m × 0. 53 mm,3. 0 μm), the detector was FID with nitrogen as the carrier gas, the detector temperature was 250 ℃ and the injector temperature was 200 ℃. Results:The linear range of dichloromethane, methanol and ethanol was 2. 436-21. 924(r=0. 998 8), 12. 268-110. 412(r=0. 999 5) and 20. 052-180. 468 μg·ml-1(r=0. 996 9) with the average recovery of 99. 30% (RSD=2. 36%), 100. 21%(RSD=1. 07%) and 100. 15%(RSD=1. 21%)(n=9), respectively. Conclusion:The detection method is sensitive, accurate and reliable, and can be used in the quality control of fenticonazole nitrate.
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Objective:To establish a method to determine the residual solvents in salvianolic acid B. Methods: The headspace GC was carried out on an HP-5 capillary column(30 m × 0. 32 mm,0. 6 μm). The inlet temperature was 180℃. The injection volume was 0. 1ml and the separation ratio was 1:10. The column temperature was programmed:the initial temperature was 40℃, malntalned for 6 min, ralsed to 180℃ with a rate of 15 ℃·min-1 , and malntalned for another 5 min. The detector was FID with the temperature of 250℃. The carrier gas was N2 with the flow rate of 1. 7 ml·min-1 . DMSO was used as the solvent for salvianolic acid B. Results:All solvents could be separated completely. The linear range of ethanol, acetone and ethyl acetate was 12. 650-1. 012 × 103 μg·ml-1 (r=0.999 3),12.750-1.012 ×103 μg·ml-1(r=0.999 7) and 12.550-1.004 ×103 μg·ml-1(r=0.999 7), respectively. The average recovery of ethanol, acetone and ethyl acetate was 96. 89% (RSD=3. 81%,n=9), 99. 56% (RSD=4. 05%,n=9) and 97. 21% (RSD=4. 95%,n=9), respectively. Conclusion:The method is simple, reproducible and accurate enough for the determi-nation of residual solvents in salvianolic acid B.
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Objective:To improve the determination method for the residual solvents in olsalazine sodium. Methods:1,2-Dichlo-roethane and chloroform were determined by headspace GC with a DB-624 capillary column and an FID detector. The column tempera-ture was 110℃. The temperature of the injector and the detector was 200℃ and 250℃, respectively. The carrier gas was nitrogen with a flow of 3. 0 ml·min-1 . The split ratio was 1∶1. Water was used as the solvent. Results:1,2-Dichloroethane and chloroform were completely separated with good linearity within the respective range of 0. 25-2. 52 ( r =0. 999 5 ) and 2. 28-22. 84 μg · ml-1 ( r =0. 999 5). The average recoveries were 98. 4% and 99. 5% with RSD of 1. 14% and 0. 98%(n=9), respectively. The detection lim-it were 0. 02 and 0. 06 μg·ml-1 , respectively. Conclusion:The method is rapid, sensitive and accurate, which can be used in the determination of residual organic solvents in olsalazine sodium.
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Objective:To establish a determination method for 8 residual organic solvents in spironolactone by capillary GC. Methods:The determination of methanol, ethanol, acetone and tetrahydrofuran in spironolactone dissolved in dimethyl sulfoxide was carried out on a DB-624 column. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The constant pressure was 2. 5psi. The column temperature was raised by program. The vial temperature was 85℃ and the time was 30min. The determination of triethylamine, pyridine, N,N-dimethylformamide and dimethyl sulfoxide in spironolactone dissolved in chloroform was carried out on an HP-1 column. The inlet temperature was 220℃ and the FID detector temperature was 250℃. The column temperature was raised by program. The flow rate of carrier gas was 3. 0ml·min-1. Results: All peaks could be separated from each other with promising resolution. The linearity of the eight solvents was fairly good(r > 0. 999). The average recovery ranged from 90. 9%-94. 3% with RSD of 1. 1%-3. 3% (n = 9). The limit of detection for methanol, ethanol, acetone, tetrahydrofuran, triethylamine, pyridine, N,N-dimethylformamide and dimethyl sulfoxide was 0. 60, 0. 67, 0. 20, 0. 15, 0. 64, 0. 36, 0. 89 and 0. 82 μg · ml-1 , respectively. Conclusion: The methods can be applied in the determination of 8 residual organic solvents in spironolactone.
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Objective: To establish a new method for determining residual organic solvent DMF in imiquimod. Methods: The samples were injected into an Agilent HP-PLOT/Q capillary column(30 m × 0. 530 mm,40. 0 μm) by a headspace sampler and ana-lyzed with an FID detector, the carrier gas was nitrogen, the inlet temperature was 250℃, and the detector temperature was 270℃. The column temperature was programmed raised. Results: The resolution among the peaks of DMF and the other residual solvents could meet the requirements. There was a good linearity within the experimental concentration range. The average recovery was 94. 6%(RSD=4. 0%, n=9). The limit of quantification and the limit of detection was 4. 809μg·ml-1 and 0. 963μg·ml-1, respectively. Conclusion:The method is convenient, accurate and sensitive, which can be used in the determination of residual solvent DMF in imi-quimod.