ABSTRACT
OBJECTIVE:To establish a method for the simultaneous determination of 6 kinds of residual organic solvents in Omeprazole magnesium,such as methanol,isopropanol,acetonitrile,dichloromethane,ethyl acetate and toluenein. METHODS:Headspace GC was adopted. The determination was performed on the column of DB-624 column by temperature programming. The inlet temperature was 200 ℃,and hydrogen flame ionization detector was adopted with the temperature of 250 ℃;nitrogen gas was used as carrier gas with flow rate of 2.0 mL/min;the splitting-radio was 5 : 1,and sample size was 1 mL;the headspace tem-perature was 80 ℃ and the equilibrium time was 20 min. RESULTS:The linear range were 12.56-628.00 μg/mL for methanol(r=0.9997),20.22-1011.20 μg/mL for isopropanol(r=0.9999),1.96-97.76 μg/mL for acetonitrile(r=0.9997),3.10-154.88 μg/mL for dichloromethane(r=0.9998),20.69-1034.56 μg/mL for ethyl acetate(r=0.9998),and 3.53-176.72 μg/mL for toluene(r=0.9998);the limits of quantitation were 1.00,0.91,0.47,0.93,0.41 and 0.35 μg/mL respectively;the limits of detection were 0.31,0.30,0.14,0.31,0.12 and 0.11 μg/mL respectively;RSDs of precision,stability and reproducibility tests were lower than 3%;the recoveries were 94.53%-101.29%(RSD=2.15%,n=9),97.78%-103.42%(RSD=1.77%,n=9),96.99%-105.76%(RSD=2.59%,n=9),96.83%-102.05%(RSD=1.86%,n=9),97.98%-101.13%(RSD=0.88%,n=9)and 97.80%-102.40%(RSD=1.41%,n=9). CONCLUSIONS:The method is sensitive and accurate,can be used for the simultaneous determination of 6 kinds of residual organic solvents in Omeprazole magnesium,such as methanol,isopropanol,acetonitrile,dichloromethane,eth-yl acetate and toluenein.
ABSTRACT
OBJECTIVE:To establish the method for simultaneous determination of 6 residual organic solvents in Xingnaojing injection,such as methanol,ethanol,isopropanol,n-butanol,ethyl acetate and acetonitrile.METHODS:Headspace GC method was adopted.The determination was performed on DB-624 capillary column by temperature programming with the injector temperature of 200 ℃;flame ionization detector was adopted with the temperature of 250 ℃;carrier gas was nitrogen with flow rate of 25 mL/min and split ratio of 35 ∶ 1;headspace sampling size was 1 mL,and heating temperature of headspace sampling was 80 ℃;equilibrium time was 15 min.RESULTS:The linear ranges of methanol,ethanol,isopropanol,n-butanol,ethyl acetate and acetonitrile were 15.00-240.00 μg/mL (r =0.999 9),25.00-400.00 μg/mL (r =0.999 9),25.00-400.00 μg/mL (r =0.999 9),25.00-399.99 μg/mL(r=0.999 9),25.00-399.99 μg/mL(r=0.999 8) and 5.00-80.00 μg/mL(r=0.999 9).The LOQ were 5.98,3.94,2.05,2.13,1.39,1.24 μg/mL,and the LOD were 2.01,2.11,1.18,1.56,1.15,0.01 μg/mL,respectively.RSDs of precision tests were all less than 2.0％,stability and repetitive tests only ethyl acetate was detected,RSD＜2.0％;the recoveries were 93.59％-99.02％ (RSD=2.62％,n=6),92.42％-98.40％ (RSD=2.43％,n=6),94.81％-104.64％ (RSD=3.47 ％,n=6),94.56％-106.73％ (RSD=4.21％,n=6),97.04％-106.33％(RSD=3.50％,n=6)and 98.40％-107.97％ (RSD=3.37％,n=6).CONCLUSIONS:The method is specific,rapid,simple and accurate,and can be used for simultaneous determination of 6 residual organic solvents in Xingnaojing injection.
ABSTRACT
OBJECTIVE:To establish the method for simultaneous determination of 6 residual organic solvents in Xingnaojing injection,such as methanol,ethanol,isopropanol,n-butanol,ethyl acetate and acetonitrile.METHODS:Headspace GC method was adopted.The determination was performed on DB-624 capillary column by temperature programming with the injector temperature of 200 ℃;flame ionization detector was adopted with the temperature of 250 ℃;carrier gas was nitrogen with flow rate of 25 mL/min and split ratio of 35 ∶ 1;headspace sampling size was 1 mL,and heating temperature of headspace sampling was 80 ℃;equilibrium time was 15 min.RESULTS:The linear ranges of methanol,ethanol,isopropanol,n-butanol,ethyl acetate and acetonitrile were 15.00-240.00 μg/mL (r =0.999 9),25.00-400.00 μg/mL (r =0.999 9),25.00-400.00 μg/mL (r =0.999 9),25.00-399.99 μg/mL(r=0.999 9),25.00-399.99 μg/mL(r=0.999 8) and 5.00-80.00 μg/mL(r=0.999 9).The LOQ were 5.98,3.94,2.05,2.13,1.39,1.24 μg/mL,and the LOD were 2.01,2.11,1.18,1.56,1.15,0.01 μg/mL,respectively.RSDs of precision tests were all less than 2.0％,stability and repetitive tests only ethyl acetate was detected,RSD＜2.0％;the recoveries were 93.59％-99.02％ (RSD=2.62％,n=6),92.42％-98.40％ (RSD=2.43％,n=6),94.81％-104.64％ (RSD=3.47 ％,n=6),94.56％-106.73％ (RSD=4.21％,n=6),97.04％-106.33％(RSD=3.50％,n=6)and 98.40％-107.97％ (RSD=3.37％,n=6).CONCLUSIONS:The method is specific,rapid,simple and accurate,and can be used for simultaneous determination of 6 residual organic solvents in Xingnaojing injection.
ABSTRACT
OBJECTIVE:To establish a method for the determination of ethanol,acetonitrile,dichloromethane,ethyl acetate, pyridine in vidarabine monophosphate. METHODS:Headspace GC was performed on the column of Agilent DB-624,programmed temperature,inlet temperature was 200 ℃,the detector was flame ionization detector,detecting temperature was 250 ℃,nitrogen was carrier gas,flow rate was 3 ml/min,split ratio was 1∶1,the top bottles equilibrium temperature was 100 ℃,and equilibrium time was 45 min,injection volume was 1 ml. external standard was used for quantitative analysis. RESULTS:The peaks of five re-sidual solvents could be completely separated from the other peaks respectively,The linear rang was 24.7-296.3 μg/ml for ethanol (r=0.999 6)、1.9-23.2 μg/ml for acetonitrile(r=0.999 0),2.8-33.6 μg/ml for dichloromethane(r=0.998 0),24.7-295.9 μg/ml for ethyl acetate(r=0.999 5),1.0-11.9 μg/ml for pyridine(r=0.998 6);RSDs of precision and reproducibility tests were lower than 4.35%;recoveries were 102.4%(RSD=2.0%,n=9)、102.1%(RSD=3.4%,n=9)、105.5%(RSD=4.8%,n=9)、100.3%(RSD=4.8%, n=9)、98.3%(RSD=4.0%,n=9). The minimum quantifation limit was 0.304 4-0.988 0 μg/ml and the minimum detection limit was 0.101 5-0.329 3 μg/ml. CONCLUSIONS:The method is simple,accurate and reproducible,and can be used for the determination of residual solvents in vidarabine monophosphate.
ABSTRACT
OBJECTIVE:To establish a method for the content determination of menthanol in Qinagli pipa syrup. METHODS:Headspace GC was performed on the column of HP-INNOWax capillary column,column temperature was 80 ℃,temperature inlet sample was 150 ℃,the detector was hydrogen flame ionization detector with temperature of 250 ℃,the flow rate of nitrogen was 0.8 ml/min with constant flow and no split,the volume injection was 1 ml,the equilibrium temperature of headspace bottle was 80 ℃,and the equilibrium time was 20 min. RESULTS:The linear range of menthanol was 2.486-24.86 μg/ml(r=0.9999),RS-Ds of precision,stability and reproducibility tests were lower than 2%,recovery was 95.4%-99.8%(RSD=1.5%,n=9). CON-CLUSIONS:The method is simple and accurate,and can be used for the content determination of menthanol in Qinagli pipa syrup.
ABSTRACT
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.
ABSTRACT
OBJECTIVE:To establish the method for the residues determination of 5 organic solvents in teicoplanin raw materi-al and injection. METHODS:Headspace GC was performed on the column with 6% cyanopropylphenyl-94% dimethyl polysiloxane (DB-624)as the stationary phase capillary column,the carrier gas was nitrogen,using the temperature program. The temperature of inlet was 200 ℃,detector was hydrogen flame ionization detector with the flow rate of 1 ml/min,split ratio was 40 ∶ 1 and the vol-ume was 1 ml. RESULTS:Good linearity of ethanol,acetone,ethyl acetate,tetrahydrofuran and triethylamine were obtained(r were 0.999 0-0.999 3);the average recoveries were respectively 95.6%,97.0%,103.2%,94.3%and 98.2%(RSD were 2.1%-4.9%, n=9);RSDs of precision and repeatability tests ≤2.6%;and the minimum detectable concentration were respectively 2,2,2,0.7 and 0.3 μg/ml. CONCLUSIONS:The established method is rapid,sensitive and accurate,and can be used for the residues determi-nation of organic solvents in teicoplanin raw materials and injection.
ABSTRACT
Objective:To establish a headspace GC method for the determination of 7 kinds of residual solvents in bicalutamide, including dichloromethane, n-hexane, tetrahydrofuran, ethanol, ether, acetone and ethyl acetate. Methods: The residual solvents in the substance were determined by GC equipped with an FID detector and linked with an Agilent DB-624 capillary column (30. 0 m × 0. 25 mm × 1. 4 m). The inlet temperature was 200℃ and the FID detector temperature was 250℃. The column temperature was raised by program:the initial temperature was 35℃, maintained for 13 min, raised to 180℃ with a rate of 100℃/min, and maintained for 5 min. The carrier gas was nitrogen and the flow rate was 1. 2 ml·min-1. The heated temperature of the headspace oven was 90℃, the heated time lasted 30 min, and the injection volume was 1. 0 ml. The solution medium was dimethyl sulphoxide (DMSO). Results:Each solvent could be completely separated, and the calibration curve of each solvent showed good linear relationship with good accuracy. Conclusion:The method can be applied for the determination of residual solvents in bicalutamide.
ABSTRACT
Objective:To establish a method for determining three residual organic solvents in nimodipine liposomes. Methods:The samples were injected into a DB-624 capillary column (30 m × 0. 32 nm,1. 8 μm) by a headspace sampler and analyzed with an FID detector, the carrier gas was nitrogen, the injector temperature was 250℃, and the detector temperature was 250℃. The column temperature was programmed raised. Results:Three residual solvents, namely ethanol, acetone and acetic ether were completely sepa-rated. There was a good linearity within the experimental concentration range. The average recovery was 98. 9%,98. 5% and 99. 4%(RSD=0. 32%,1. 12%,0. 76%,n=9), respectively. The detection limits was 0. 20, 0. 18 and 0. 22μg·ml-1, respectively . Con-clusion:The method is rapid, sensitive and accurate. It can be used in the determination of residual organic solvents in nimodipine li-posomes.
ABSTRACT
This study was aimed to analyze the volatile oil of Mentha crispata Schrad. ex Willd. in order to provide evidence for its chemotype and guidance for its production application. The chemical analysis was detected by headspace GC-MS. The results showed that 64 chemical compounds were detected. It was concluded that the volatile oil of M. crispata Schrad. ex Willd. mainly contained eucalyptol (35.58%), limonene (16.92%) and pinene (15.33%). It was concluded that the analysis on composition characteristics and main compounds of M. crispata Schrad. ex Willd. can provide evidences in its production application and chemotype.
ABSTRACT
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.
ABSTRACT
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.
ABSTRACT
Objective To evaluate the measurement uncertainty for the determination of ethanol in human blood by auto-headspace GC/MS.Methods Each source of uncertainty,arising from the procedure of testing,was analyzed and confirmed according to the guidelines of the uncertainty in measurement.After each uncertainty component was evaluated,the combined standard uncertainty and the expanded uncertainty of the result were calculated.Results The expanded uncertainty was 0.084mg/mL when the concentration of ethanol in blood sample was 0.738 mg/mL.Conclusion The measurement uncertainty of the concentration of ethanol was came primarily from the sample determination,standard solution of the ethanol and the calibration curve.
ABSTRACT
Objective:To establish a method for analysis of residual organic solvents (methanol, ethanol, acetone, ethyl acetate) in Ginkgo biloba Leaves for injection.Methods: The contents of residual solvents in Ginkgo biloba Leaves for injection were determined by headspace GC on HP 5 column, with FID detector, high purity nitrogen as the carries gas.Results: There was a good linearity ( r :0.9909～0.9999). The RSD of precision and accuracy was less than 5%, the average recovery rate was in the range of 93.06%～113.78%.Conclusions: The method was simple, quick and accurate and can be used for quality control of Chinese patent medicine.
ABSTRACT
OBJECTIVE:To develop a headspace GC method for determination of residual organic solvents invovling methanol,alcohol,acetone,acetonitrile,dichloromethane and n-butanol in meropenem.METHODS:The residual organic solvents were separated on DB-624 capillary column using temperature programming.FID was used as detector with a temperature of 250 ℃ with nitrogen as carrier gas and water as solvent.The inlet temperature was 200 ℃.RESULTS:The linear range were 12～600 ?g?mL-1 (r=0.999 8) for methanol,20～1 000 ?g?mL-1 (r=0.999 9) for alcohol,20～1 000 ?g?mL-1 (r=0.999 9) for acetone,1.64～82 ?g?mL-1 (r=0.999 8) for acetonitrile,2.4～120 ?g?mL-1 (r=0.999 6) for dichloromethane and 20～1 000 ?g?mL-1 (r=0.999 9) for n-butanol with RSD of 1.0%,2.2%,0.9%,2.2%,1.6%,1.1%,respectively.The average recoveries were ranged from 98.8% to 99.6%.The LOD were about 0.06～0.43 ng.The residual levels of six organic solvents in 3 batches samples were all up to the standard stated in Chinese Pharmacopeia (2005 edition).CONCLUSION:The method is simple,accurate,sensitive and reproducible for determination of residual organic solvents in meropenem.