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OBJECTIVE： To establish a method for simultaneous determination of 9 kinds of organic solvents residues in total flavonoids extracts from Abelmoschus manihot. METHODS： Headspace GC was adopted to determine the contents of 9 kinds of organic solvents residues in total flavonoids extracts from A. manihot， such as benzene， acrylonitrile， methyl methacrylate， toluene， 1，2-dichloroethane， xylene， chlorobenzene， styrene and divinylbenzene. The determination was performed on Agilent DB-WAX capillary column （30 m×0.25 mm， 0.25 μm） through temperature-programmed route. The inlet temperature and FID detector temperature were set at 250 ℃. The carrier gas was nitrogen with the flow rate of 1.2 mL/min. The split ratio was 10 ∶ 1. The containers of headspace injector were in equilibrium at 90 ℃ for 45 min and the sample size was 1 mL. RESULTS： The separation degree among the peaks of 9 components was greater than 1.5， and the blank solvent （10％ N-methyl pyrrolidone aqueous solution） had no interference. The linear ranges of them were 0.16-1.21， 0.80-6.03， 1.61-12.09，1.62-12.12， 0.16-1.21， 1.60-12.01， 0.81-6.11， 1.60-12.03， 0.80-6.03 μg/mL， respectively （r≥0.999 4）. The limits of quantitation were 0.162 08， 0.201 08， 0.080 6， 0.080 768， 0.161 92， 0.400 36， 0.040 712， 0.026 736， 0.013 395 μg/mL； the limits of detection were 0.040 52， 0.040 216， 0.026 87， 0.026 9，0.040 48， 0.080 072， 0.013 57， 0.008 912， 0.004 465 μg/mL， respectively. RSDs of precision （n＝5） and reproducibility （n＝6） tests were all lower than 5％. Average recoveries were 99.41％-111.27％（RSD＜9％， n＝9）. Above 9 residual solvents were not detected in 3 batches of total flavonoids extracts from A. manihot. CONCLUSIONS： Established method is simple， accurate and reliable， and can be applied for simultaneous detection of 9 kinds of organic solvents residues in total flavonoids extracts from A. manihot.
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A simple and sensitive method for simultaneous determination of 12 kinds of residual solvents in a new drug CBT108 was established and validated by headspace gas chromatographic technology. The rationality,accuracy and feasibility of the analytical method were verified. Under the optimized conditions, simultaneous separation and determination of 12 kinds of residual solvents, including methanol, ethanol, ether, acetone, acetonitrile, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, heptane, toluene and carbon tetrachloride was carried out by using a DB624 capillary column(30 m×0.53 mm×3.0 μm) for separation, a flame ionization detector for detection and internal standard method for quantitation. Good linearity was obtained for 12 solvents with the correlation coefficients(R2) of more than 0.997. The limits of quantitation and detection were defined at S/N=3 and S/N=10,respectively. LOQ and LOD for 12 solvents were given as 0.024 μg/mL and 0.0072 μg/mL for methanol,0.1 μg/mL and 0.012 μg/mL for ethanol, 0.01 μg/mL and 0.005 μg/mL for ether, 0.1 μg/mL and 0.008 μg/mL for acetone, 1.025 μg/mL and 0.0615 μg/mL for acetonitrile, 0. 09 μg/mL and 0. 06 μg/mL for dichloromethane, 0. 09 μg/mL and 0.06 μg/mL for n-hexane, 0. 25 μg/mL and 0. 008 μg/mL for ethyl acetate, 0. 108 μg/mL and 0.014 μg/mL for tetrahydrofuran,0.16 μg/mL and 0.0004 μg/mL for carbon tetrachloride,0.0075 μg/mL and 0.005 μg/mL for heptane, and 0.0445 μg/mL and 0.0014 μg/mL for toluene. The adding standards recoveries for 12 residual solvents at three spiked levels were in the range of 90.96%-108.67%,with relative standard deviations of 0.1%-5.7%. This simple,high accuracy and good repeatability method is feasible for rapidly determination of 12 residual solvents in drug candidate CBT108. Meanwhile, this simple method provides a consulted value for detection of residual solvents in other medicines.
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A headspace gas chromatography method was developed for the determination of six residual solvents including methanol, ethanol, acetone, dichloromethane, tetrahydrofuran and toluene residues in selexipag to provide the experimental basis for its quality control.The samples were separated on Kromat PC-624(V)silica capillary column(30.0 m ×0.32 mm,1.8 μm)using temperature programming.The column temperature was kept at 40 ℃ for 5 min initially,and then raised to 180 ℃ at the rate of 20 ℃ /min and subsequently sustained for 5 min.FID detector temperature was 250 ℃ and injection temperature was 200 ℃.The split ratio was 20 : 1. The six residual solvents are separated completely under the given chromatographic conditions with a good linearity (r=0.998 2-1.000);the results of precision,repeatability and stability experiments met the requirement,and the mean recoveries of all solvents were in the range of 96.67％-101.7％.The analytical method is simple,accurate and sensitive,and it can be used for the determination of residual solvents in selexipag.
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OBJECTIVE:To establish a method for simultaneous determination of 4 residual organic solvents such as ethanol,dichloromethane,isopropanol and ethyl acetate in lacidipine raw material.METHODS:GC method was adopted.The determination was performed on DB-624 capillary column at the rate of 2.0 mL/min using nitrogen gas as carrier and FID as the detector by temperature programming.The temperature of detector was set at 250 ℃.Carries gas was nitrogen.The split ratio was 10 ∶ 1.The sample size was 10 μL.RESULTS:The linear ranges of ethanol,dichloromethane,isopropanol and ethyl acetate were 0.259 5-2.076 mg/mL (r=0.999 6),0.055 3-0.316 mg/mL (r=0.999 2),0.342 3-1.956 mg/mL (r=0.999 5),0.370 6-2.118 mg/mL(r=0.999 4),respectively.The limits of quantification were 2.96,2.24,4.4,4.44 μg/mL,and the detection limits were 0.887,0.672,1.3,1.32 μg/ mL,respectively.RSDs of precision,stability and reproducibility tests were all lower than 4.0％.The recoveries were 95.00％-101.17％ (RSD=2.19％,n=9),96.22％-104.53％ (RSD=3.27％,n=9),96.20％-104.90％ (RSD=2.41％,n=9),95.60 ％-104.48 ％ (RSD=2.85 ％,n=9).CONCLUSIONS:The method is simple,sensitive and reliable,and is suitable for simultaneous determination of 4 residual organic solvents in lacidipine raw material.
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Objective:To determine the content of cyclohexane, ethyl acetate, methanol, methylene chloride and trichloromethane in rupatadine fumarate by headspace gaschromatography. Methods:A DB-WAXETRR capillary column(30 m × 0. 32 mm,0. 25 μm)was used and the carrier gas was nitrogen. The detector was an FID and the inlet temperature was 200℃ . The column temperature program was with the initial temperature of 35℃,maintained 10 min,and then risen to 220℃ with the rate of 20℃·min -1 ,and maintained 5 min. Results:Cyclohexane,ethyl acetate,methanol,methylene chloride and trichloromethane showed a good linear relationship within the range of 77. 590 1- 698. 310 9 μg·ml -1(r = 0. 999 7),102. 166 6- 919. 499 4 μg· ml -1(r = 0. 999 8),62. 744 7- 564. 703 2μg·ml -1(r = 0. 999 9),12. 011 2- 108. 101 1 μg·ml-1(r = 0. 999 6)and 1. 262 8-11. 365 6 μg·ml -1(r = 0. 999 6). The average recovery was 103. 9% ,103. 5% ,104. 9% ,107. 1% and 103. 4% and RSD was 2. 3% ,2. 6% ,3. 1% ,2. 8% and 4. 5%(n = 9),respectively. The five residual solvents were not detected out in rupatadine fumarate. Conclusion:The method is stable,simple,sensitive and accurate,and can be used for the determination of residual solvents in rupatadine fumarate.
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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.
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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.
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OBJECTIVE:To establish a method for determining residual solvents in Decitabine for injection. METHODS:Cap-illary GC method was adopted,and the contents of residual solvents were calculated by internal standard method. The column was capillary column Agilent DB-624,flame ionization detector was used with the temperature of 280 ℃ by temperature programming, and the temperature of injector was 230 ℃,nitrogen was used as the carrier gas,flow rate was 1.5 ml/min and the split ratio was 50:1,direct injection was used,and the sample size was 1 μl. RESULTS:The linear range was 0.100 3-2.507 mg/ml for ethanol , 0.101 3-2.532 mg/ml for ether,0.102 2-2.556 mg/ml for isopropanol,0.008 3-0.207 8 mg/ml for acetonitrile,0.012 4-0.309 3 mg/ml for methylene chloride,0.014 8-0.369 4 mg/ml for tetrahydrofuran,0.078 1-1.953 mg/ml for cyclohexane,0.024 9-1.250 mg/ml for toluene and 0.017 6-0.440 9 mg/ml for N,N-dimethylformamide(r≥0.999 2);RSDs of precision and reproducibility tests were lower than 2%;recovery was 96.70%-101.60%(RSD was 0.59%-1.82%,n=9). CONCLUSIONS:The method is simple,accurate and reproducible and suitable for determining the residual solvents in Decitabine for injection.
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OBJECTIVE:To establish the method for determining 10 residual organic solvents in norvancomycin hydrochloride raw material. METHODS:Headspace gas chromatography was performed on the column of nitro modified polyethylene terephthal-ate glycol as stationary phase capillary column;the oven temperature program started at 40 ℃ for 3 min and increased at a rate of 8 ℃/min up to 150 ℃ for 10 min;the temperature was 200 ℃ with carrier gas of high-purity nitrogen gas,the constant flow rate was 5 ml/min with split ratio of 15∶1;the headspace vial equilibrium temperature was 85 ℃ with equilibrium time of 40 min,and the volume was 1 ml. RESULTS:The concentration of n-pentane,acetone,ethanol,benzene,acrylonitrile,toluene,xylene,chlo-robenzene,styrene,divinylbenzene had good linear relationship with its peak area values(r=0.995 7-0.999 9);the RSDs of preci-sion,repeatability tests was ≤6.6%;average recovery was in the range of 94.3%-106.6%(RSD=0.5%-4.5%,n=9). CONCLU-SIONS:The method is fast,sensitive and accurate,and can be used for the determination of residual organic solvents in norvanco-mycin hydrochloride raw material.
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An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chroma-tograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB-624 (30 m × 0.53 mm i.d., 3.00μm film thickness) column was used. The inlet split ratio was 5:1. The influ-encing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were 30 °C for IT, 158 °C for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents through a comprehensive validation according to the ICH guidelines.
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To develop a method for the determination of residual solvents inα-ketophenylalanine calcium by capillary gas chromatography. Methods:The residual solvents were separated on a DB-624(30 m × 0. 32 mm, 0. 25 μm) capillary chromato-graphic column with temperature programming. The column temperature was maintained at 40℃ for 1 min,and then raised to 180℃at a rate of 10℃·min-1 and maintained for 2 min. N2 was used as the carrier gas, and FID was used as the detector with temperature of 250 ℃. The injector temperature was 200 ℃ and the split ratio was 10∶1, and direct injection was adopted. Methanol, ethanol, ethyl acetate and tetrahydrofuran in α-ketoleucine calcium were detected using an external standard method. Results:The four solvents were separated completely. There was a good linear relationship between the peak area and the concentration of each solvent ( r=0. 997 2-0. 999 5). The average recovery of the four solvents was 95. 47%-100. 26%(RSD≤4. 7%, n=9). Conclusion:The method is rap-id, simple, accurate and sensitive, and can be used in the determination of residual solvents in α-ketophenylalanine calcium.
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Objective:To establish a headspace capillary GC method for the determination of residual solvents in bromfenac sodi-um. Methods:A headspace GC was used to separate the residual solvents on an HP-5 capillary column with an FID detector. The car-rier gas was nitrogen at the flow rate of 0. 8 ml·min-1 . The temperature of the injector was 200 ℃ and that of the FID was 250 ℃. The programmed column temperature was set as follows:maintained at 40℃ for 10 min, and then raised to 150℃ at the rate of 30℃·min-1 and maintained for 5 min. The containers of headspace injector were in equilibrium at 100 ℃ for 20 min. Dimethyl sulfoxide was used as the solvent. The amount of the residual solvents, such as methylbenzene, isopropanol, dichloromethane, methanol and iso-propyl ether was calculated by an external standard method. Results:All the solvents could be completely separated with good linear relationship. The average recovery of the five solvents was 98. 9%( RSD =2. 01%),99. 2% ( RSD =1. 95%),99. 6% ( RSD =1. 65%),100. 5%(RSD=1. 38%)and 100. 8%(RSD=1. 36%)(n=9),respectively. Conclusion:The method is simple and accu-rate in the determination of the five residual solvents in bromfenac sodium.
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Objective To establish a capillary gas chromatography( GC)method for the determination of residual organic solvents in poly( lactic-co-glycolide)( PLGA),including methanol,acetone,dichloromethane,and toluene. Methods A capillary GC method was carried out. DB-624 capillary column(30 m× 0. 32 mm,1. 80 μm)with programmed temperature chromatography was employed. The initial temperature was kept at 40 ℃ for 8 min. Then the temperature was raised to 200 ℃ at a rate of 10 ℃·min-1 . The injection port temperature was 180 ℃,and the split ratio was 10:1. The carrier gas was nitrogen. The temperature of FID was set at 250 ℃,and the sample volume was set at 3 μL. Results Four residual organic solvents consisting of methanol,acetone,dichloromethane and toluene in PLGA were completely separated. The linear range of concentration of methanol,acetone,dichloromethane and toluene was within 10. 0-50. 0( r=0. 999 8 ),16. 7-83. 3( r=0.9998),2.0-10.0(r=0.9993),and3.0-14.8(r=0.9997)μg·mL-1,respectively.Therecoveryofmethanol,acetone, dichloromethane and toluene was 99. 9%( RSD=1. 5%),100. 8%( RSD=0. 9%),100. 1%( RSD=1. 1%),and 99. 5%(RSD=0. 6%),respectively. Six batches of samples met the requirements. Conclusion The method is proven to be sensitive and accurate after the validation. It is suitable for the determination of residual organic solvents in PLGA.
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Naproxen, an anti-inflammatory drug, exhibits poor aqueous solubility, which limits the pharmacological effects. The present work was carried out to study the effect of agglomeration on micromeritic properties and dissolution. Naproxen agglomerates were prepared by using a three solvents system composed of acetone (good solvent), water (non-solvent) and dichloromethane (bridging liquid). Differential Scanning Calorimetry (DSC) results showed no change in the drug after crystallization process. X-Ray Powder Diffraction (XRPD) studies showed the sharp peaks are present in the diffractograms of spherical agglomerates with minor reduction in height of the peaks. The residual solvents are largely below the tolerated limits in the agglomerates. Scanning Electronic Microscopy (SEM) studies showed that agglomerates were spherical in structure and formed by cluster of small crystals. The agglomerates exhibited improved solubility, dissolution rate and micromeritic properties compared to pure drug. Anti-inflammatory studies were conducted in Wistar strain male albino rats and naproxen agglomerates showed more significant activity than the pure drug.
Naproxeno, fármaco anti-inflamatório, apresenta baixa solubilidade em água, o que limita os efeitos farmacológicos. O presente trabalho foi realizado para estudar o efeito da aglomeração nas propriedades micromeríticas e na dissolução. Aglomerados de naproxeno foram preparados por meio da utilização de sistema de três solventes composto de acetona (bom solvente), água (não-solvente) e diclorometano (líquido de ligação). A DSC não resulta mostrou nenhuma mudança na droga depois de processo de cristalização. Estudos de difração de Raios X do Pó (XRPD) mostraram picos agudos nos difratogramas de aglomerados esféricos, com redução mínima dea altura dos picos. Os solventes residuais estão amplamente abaixo dos limites tolerados nos aglomerados. Os estudos de Microscopia Eletrônica de Varredura (SEM) mostraram que esses aglomerados eram de estrutura esférica e formados por grupos de pequenos cristais. Os aglomerados apresentaram solubilidade, taxa de dissolução e propriedades micromeríticas aprimoradas em comparação com o fármaco puro. Estudos anti-inflamatórios foram conduzidos em ratos Wistar albinos masculinos e os aglomerados de naproxeno mostraram atividade mais significativa do que o fármaco puro.
Subject(s)
Dissolution/methods , Naproxen/analysis , Anti-Inflammatory Agents/pharmacokinetics , Calorimetry, Differential Scanning/classification , Methylene Chloride/analysis , Solvents/classificationABSTRACT
Residual solvents in pharmaceutical samples are monitored using gas chromatography with head space. Based on good manufacturing practices, measuring residual solvents is mandatory for the release testing of all active pharmaceutical ingredients (API). The analysis of residual organic solvents (methanol, acetone, cyclohexane, dichloromethane, toluene) in Omeprazole, an active pharmaceutical ingredient was investigated. Omeprazole is a potent reversible inhibitor of the gastric proton pump H+/K+-ATPase. The Head space gas chromatography (HSGC) method described in this investigation utilized a SPB TM-624, Supelco, 30 m long x 0.25 mm internal diameter, 1.4µm-thick column. Since Omeprazole is a thermally labile compound, the selection of the proper injector temperature is critical to the success of the analysis. The injector temperature was set at 170ºC to prevent degradation. The initial oven temperature was set at 40ºC for 12 min and programmed at a rate of 10ºC min-1 to a final temperature of 220ºC for 5 min. Nitrogen was used as a carrier gas. The sample solvent selected was N,N-dimethylacetamide. The method was validated to be specific, linear, precise, sensitive, rugged and showed excellent recovery.
Solventes residuais em amostras farmacêuticas são monitoradas utilizando-se cromatografia a gás "headspace". Com base nas boas práticas de fabricação, a medida de solventes residuais é obrigatória para o teste de liberação de todos os ingredientes farmacêuticos (API). Efetuou-se a análise de solventes orgânicos residuais (metanol, acetona, cicloexano, diclorometano, tolueno) em omeprazol, ingrediente farmacêutico ativo. O omeprazol é potente inibidor reversível da bomba de prótons H+/K+-ATPase. A cromatografia a gás "headspace" (HSGC) descrita nessa pesquisa utilizou um SPB TM-624, Supelco, de 30 m de comprimento x 0,25 mm de diâmetro interno, e coluna de 1,4 µm de espessura. Considerando-se que o omeprazol é termicamente lábil, a seleção da temperatura apropriada do injetor é crítica para impedir a degradação. A temperatura inicial do forno foi de 40 ºC, por 12 minutos, e programada à taxa de acréscimo de 10 ºC min-1 até a temperatura final de 220 ºC, por 5 minutos. Nitrogênio foi utilizado como gás de transporte. Selecionou-se como solvente a N,N-dimetilacetamida. O método foi validado mostrando-se específico, linear, preciso, sensível, robusto e com excelente recuperação.
Subject(s)
Chromatography, Gas , Omeprazole/analysis , Omeprazole/chemistry , Solvents/chemistry , Enzyme Inhibitors/analysis , Enzyme Inhibitors/chemistry , Methodology as a SubjectABSTRACT
PURPOSE: Analysis of volatile organic solvents in 2-deoxy-2-[18F] fluoro-D-glucose ([18F]FDG) preparations was performed by gas chromatography (GC), in accordance with USP. MATERIALS AND METHODS: Analyses were carried out on a Hewlett-Packard 6890 gas chromatography equipped with an FID. RESULTS: We determined the amounts of ethanol and acetonitrile on every batch of our routine [18F]FDG preparations, ranging between 5000 ppm and 100 ppm. In our routine preparation of [18F]FDG, the amount of acetonitrile and ethanol in the final product were well below the maximum allowable limit described in the USP. CONCLUSION: Our [18F]FDG preparations were in accordance with the suggested USP maximum allowable levels of the quality control analysis of volatile organic compounds.
Subject(s)
Chromatography, Gas , Ethanol , Quality Control , Solvents , Volatile Organic CompoundsABSTRACT
OBJECTIVE:To determine the contents of the residual solvents including dichloromethane,acetone and ethanol in azithromycin raw material by GC.METHODS:A glass column was used as chromatographic column.The temperature of sample injection was 140℃and column temperature was 160℃.The carrier gas was nitrogen.The column inlet pressure was 30Psi.The detection was performed using hydrogen flame ionization detector.RESULTS:The detection concentrations of dichloromethane,acetone and ethanol were 0.02%～0.1%(r=0.9 995),0.05%～0.25%(r=0.9 994)and 0.02%～0.1%(r=0.9 994),respectively.The average recovery were 99.1%(RSD=1.4%),100.1%(RSD=1.1%)and 99.5%(RSD=1.3%),respectively.All of the three batches of samples were up to the standard with regard to the residual volume of organic solvent residues in azithromycin raw material.CONCLUSION:The method is proved to be accurate,sensitive and reliable,and suitable for the detection of organic solvent residues in azithromycin.
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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.
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AIM: To establish a method for detecting the residual solvents in protopanaxdiol. METHODS: Capillary GC with HP-PLOT-Q column (30 m ? 0. 53 mm ? 1. 0 ?m) was used to determine residual in protopanaxdiol. N,N-dimethyl-acetamide as solvent media,FID detector and nitrogen as the carrier gas. RESULTS: There was a good linearity at the experimental concentration (r = 0. 999 96-0. 999 99),the RSD of precision was less than 6. 0 % . The spotting recovery of the 3 residul,including methol,ethyl acetate and n-butanol,was in the range of 98. 2%-102. 2% ,and its’RSD was 1. 1%-2. 4% . CONCLUSION: The method is simple,accurate and of high sensitivity,can be used for the determination of residual solvents in protopanaxdiol.
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At present,there is not a clear guideline for residual solvents in the new drugs in our country. In practice,the ICH Q3C is our important reference in general,but in practical research and evaluation of new drugs,some adjustment should be made on principles of ICH Q3C,making it suitable for the reality of the pharmaceutical industry in our country. In this article, we put forward some suggestions to improve the quality control of residual solvents in our country,and some initial ideas were provided to solve the question in practice.