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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 determination of the twelve residual organic solvents,including methanol,ethanol,acetone,isopropanol,tert-Butyl methyl ether,dichloromethane,aceticether,tetrahydrofuran,triethylamine,trimethylorthofor-Mate,morpholine,N,N-Dimethylformamide in Apixaban bulks drug.Methods Gas head-space chromatography was applied to this study.The column was DB-624 silica capillary column (30.0 m × 0.53 mm × 3.00 μm) and the carrier gas was high purity nitrogen;The vial temperature was 100 ℃,and the vial time was 20 min.The Column temperature was kept at 40 ℃ for 6 min,then the temperature was raised to 220 ℃ at the rate of 20 ℃/min and subsequently sustained for 10 min.FID detector temperature and injection temperature were both 250 ℃.The N2 flow rate was 2.8 mL/min.Split ratio was 5∶1.Results Twelve kinds of solvents were completely separated and determined with a good linearity (r =0.9994-0.9999).The RSD values of precision experiments and the average recovery was in line with the requirements.Conclusion Theanalytical method is simple,accurate and sensitive,which could be used for determination of residual organic solvents in Apixaban bulks drug.
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OBJECTIVE:To establish a method for the determination of 9 residual organic solvents in blonanserin as methanol, alcohol,isopropyl alcohol,acetonitrile,dichloromethane,hexane,ethyl acetate,tetrahydrofuran and methylbenzene. METHODS:Headspace gas chromatography was adopted. The determination was performed on DB-624 capillary column using temperature pro-gramming. The inlet temperature was 150 ℃,and flame ionization detector was used with temperature of 250 ℃. High purity nitro-gen was used as carrier gas with flow rate of 2.8 mL/min. The split ratio was 1:1,and headspace sample size was 1 mL. Head-space heating temperature was 90 ℃,and equilibration time was 35 min. RESULTS:The linear ranges of methanol,alcohol,iso-propyl alcohol,acetonitrile,dichloromethane,hexane,ethyl acetate,tetrahydrofuran and methylbenzene were 6-1500 μg/mL(r=0.9998),10-2500 μg/mL(r=0.9999),10-2500 μg/mL(r=0.9998),0.82-205 μg/mL(r=0.9994),1.2-300 μg/mL(r=0.9995), 0.58-145 μg/mL(r=0.9994),10-2500 μg/mL(r=0.9999),1.44-360 μg/mL(r=0.9996),1.78-445 μg/mL(r=0.9995),respec-tively. The limits of quantitation were 17.71,6.02,3.17,7.45,1.53,0.69,0.93,1.01,0.22 μg/mL;the limits of detection were 5.89,1.90,1.05,2.48,0.51,0.23,0.31,0.33,0.07 μg/mL,respectively. RSDs of precision and stability tests were all lower than 3.0%,and isopropanol was found in repeatability test (RSD=2.1%). The average recoveries ranged 96.67%-102.66%(RSD=1.9%,n=9),96.00%-101.83%(RSD=1.9%,n=9),97.17%-101.50%(RSD=1.4%,n=9),96.97%-102.44%(RSD=2.2%,n=9),95.83%-103.33%(RSD=2.5%,n=9),95.83%-100.28%(RSD=1.9%,n=9),98.17%-101.25%(RSD=1.0%,n=9),96.55%-102.30%(RSD=1.9%,n=9),96.30%-102.22%(RSD=1.8%,n=9),respectively. CONCLUSIONS:The method is simple,rapid,accurate and suitable for simultaneous determination of 9 residual organic solvents in blonanserin as methanol,alco-hol,isopropyl alcohol,acetonitrile,dichloromethane,hexane,ethyl acetate,tetrahydrofuran and methylbenzene.
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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 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 headspace capillary gas chromatography method for the determination of residual solvents in erlotinib hydrochloride .Methods:A DB-624 capillary column (30 m ×0.53 mm, 3.0 μm) was used and the carrier gas was nitro-gen.The flow rate was 2.0 ml· min-1 and the inlet temperature was 190℃.The FID detector temperature was 230 ℃.The column temperature program was with the initial temperature of 35℃( maitaining 8 min) , risen to 170℃with the rate of 28℃· min-1 ( main-taining 8 min) , and then risen to 200℃with the rate of 32℃· min-1 ( maintaining 7 min) .The headspace vial temperature was 100℃and the time was 30 min.Results:Ethanol, isopropanol, methylene chloride and n-butanol had a good linear relationship within the range of 0.68-409.14 μg· ml-1 (r=0.999 8),0.67-404.88 μg· ml-1 (r=0.999 8),1.71-51.31μg· ml-1 (r=0.999 7) and 0.72-431.12 μg· ml-1(r=0.999 8), respectively.The average recovery was 99.0% (RSD=0.41%, n=9), 100.2%(RSD=0.52%, n=9),97.1%(RSD=1.75%, n =9) and 102.5% (RSD=1.08%, n=9), respectively.Conclusion: The method is simple and accurate , which can be used for the determination of four residual organic solvents in erlotinib hydrochloride .
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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 GC method for the determination of residual organic solvents in lidocaine patches. Methods:GC was carried out on a DB-WAX capillary column (30 m × 0. 25 mm, 0. 5 μm). The detector was FID and the carrier gas was He. The initial temperature was 50℃, maintained for 8 min, and then raised to 250℃ with a rate of 50℃ per min. The inlet temperature and the detector temperature were 280℃. The separation was 50 ∶1. Results:The linear range of acetone, ethyl acetate and methanol was 15. 0-600. 0 μg·ml-1. The average recovery was 97. 4% (RSD =3. 2%, n=9), 95. 6% (RSD=1. 9%, n=9) and 112. 0%(RSD =4. 5%, n=9), respectively. Conclusion:The method is simple and accurate,which can be used for the determination of re-sidual organic solvents in lidocaine patches.
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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 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 determine the content of chloroform, ethyl acetate and DMF in dimemorfan phosphate by gas chromatog-raphy (GC). Methods:The capillary gas chromatography was used with a PEG-20M column, programmed temperature, water as the solvent and FID as the detector. Results:The three organic solvents were separated and showed good linear relationship (r>0. 999 0). The detection limit of chloroform, ethyl acetate and DMF was 0. 63,0. 60 and 8. 92μg·ml-1 , respectively. The residues of the organ-ic solvents in three batches of the samples all met with the requirements of ICH. Conclusion: The method is sensitive, accurate and reliable, and can be used in the quality control of dimemorfan phosphate.
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Objective:To establish a capillary GC method for the determination of residual organic solvents in paclitaxel. Meth-ods:The standard solution and test solution was respectively injected into an HP-INNOWAX sillica capillary column by headspace in-jection. The chromatograms were recorded with an FID. The injection port and detector temperature was 250℃ and 300℃, respective-ly, the initial column temperature was kept at 35℃ for 5 min, and then was risen to 260℃ at the rate of 25℃/min. Results:The four residual organic solvents could be separated completely. The resolution and sensitivity were acceptable. Conclusion: The method is proved to be simple, rapid, sensitive and reliable, and can be used in the determination of residual organic solvents in paclitaxel.
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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 headspace GC method for the determination of residual organic solvents in testosterone cypionate. Methods The residual organic solvents were determined by GC with DB-WAX capillary colum(30 m× 0. 32 mm,0. 25 μm)and FID detector at 230℃,using high purity nitrogen as the carrier gas by headspace sampling. The flow rate was 1. 5 mL·min-1 ,the split ratio was 20:1,the temperature of injection port was 220℃,the headspace heating temperature was 70 ℃,and the headspace balance time was 40 mins. The content of residues was calculated by using n-propanol as the internal standard. Results Four residual solvents were completely separated. There were good linearity for m-ethanol,ethanol,benzene and pyridinein in the ranges of 4. 17-2. 50×103 μg·g-1(R=0. 999 9),4. 18-2. 51×103 μg·g-1(r=0. 999 6),0. 84-172 μg·g-1 (r=0. 998 1),and 2. 95-1. 77×103μg·g-1(r=0. 999 9),respectively. The detection limit was 2.08,1. 23,0.28,and 0. 87 μg·g-1,respectively. The average recovery of methanol,ethanol,benzene and pyridinein was 102. 2%(RSD=4. 0%),99. 6%(RSD=1. 9%),112. 6(RSD=5. 6%),and 98. 9%(RSD=1. 6%),respectively. Conclusion This method is reliable,sensitive, accurate and can be used for the determination of residual organic solvents in testosterone cypionate.
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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.
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Objective:To determine the content of methanol, alcohol and isopropanol in flupirtine maleat by headspace gas chro-matography. Methods:The capillary gas chromatography with programming temperature was established with an FID detector and a DB-624(30 m × 0. 53 mm,3. 0 μm) capillary column. The temperature of the injector and the detector was 200℃ and 250℃, respec-tively. The residual organic solvents were determined by an external standard method. Results: Methanol, alcohol and isopropanol showed good linearity within the range of 2. 182~152. 74(r=0. 999 1), 3. 546-248. 22(r=0. 9998)and 4. 082-285. 74 μg·ml-1(r=0. 999 7) with the average recovery of 97. 7%(RSD=1. 5%),99. 0%(RSD=1. 1%)and 98. 8%(RSD=1. 1%)(n=5), respec-tively. Conclusion:The method is simple, sensitive and accurate, and can be used in the residual solvents detection for flupirtine mal-eat.
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Objective:To establish a detection method for residual toluene in diclofenac sodium raw material by GC. Methods:An HP-5 column (0. 53 mm × 30 m, 2. 65 μm) with nitrogen as the carrier gas was employed for the separation. The temperature of the column, injection port and FID detector was set at 50℃, 200℃ and 250℃, respectively. An internal standard method with isooctane as the internal standard was used to assay the residual amount after the sample was dissolved in DMSO. Results:The linear calibration curve was obtained over the range of 9. 27-111. 19μg·ml-1(r=0. 999 4). The mean recovery was 97. 27%(RSD=2. 80%,n=9). The LOD and LOQ was 0. 59μg·ml-1 and 1. 46μg·ml-1 , respectively. The residual contents of toluene in 3 batches of the products all met the relevant regulations. Conclusion:The established method is reliable and accurate, and can be used in the quality control of diclofenac sodium.
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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 headspace capillary gas chromatography for the content determination of residual solvents in letrozole, such as chloroform, ethanol, acetone, ethyl acetate, DMF and isopropanol. METHODS: Dissolved in dimethyl sulfoxide, chloroform, ethanol, acetone, ethyl acetate, DMF and isopropanol in letrozole were determined by headspace gas chromatography with HP-5 capillary gas chromatography. ECD was applied for chloroform, while FID was applied for the other residual solvents. RESULTS: The liner ranges of chloroform, ethanol, acetone, ethyl acetate, DMF and isopropanol were 1.028～10.28 mg?L-1(r=0.999 9), 94.68～946.8 mg?L-1 (r=0.999 7), 94.64～946.4 mg?L-1(r=0.999 7), 110.64～1 106.4 mg?L-1(r=0.999 7), 15.12～151.2 mg?L-1(r=0.999 6), 116.48～1 164.8 mg?L-1(r=0.999 5), respectively. The average recoveries of the residual organic solvents ranged from 97% to 102%. The detection limits were 20～90 ?g?L-1. The residual levels of the six organic solvents in three batches of samples were all up to the standard stipulated in Chinese Pharmacopeia. CONCLUSIONS: The method is simple, sensitive, accurate and reliable for the content determination of residual organic solvents in letrozole.