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OBJECTIVE:To establish a method for simultaneous determination of 6 residual organic solvents in aprepitant raw material as methanol,ethanol,acetone,isopropyl alcohol,methyl tert-butyl ether and tetrahydrofuran.METHODS:Headspace capillary gas chromatography was adopted.The determination was performed on DB-624 capillary column using temperature programming.The temperature of injector port was 180 ℃,and flame ionization detector was used with temperature of 260 ℃.Nitrogen was used as carrier gas with flow rate 3.0 mL/min.The spilt ratio was 5 ∶ 1,and head-space injection volume was 1.0 mL.The head-space equilibrium temperature was set at 80 ℃,and equilibrium time was 40 min.RESULTS:The linear ranges of methanol,ethanol,acetone,isopropyl alcohol,methyl tert-butyl ether,tetrahydrofuran were 6.052-605.232 μ g/mL (r=0.999 9),9.987-998.718 μg/mL(r=0.999 9),9.998-999.768 μg/mL(r=0.999 8),9.986-998.634 μg/mL(r=0.999 9),9.991-999.090 μg/mL (r=0.999 7),1.461-146.133 μg/mL(r=0.999 5),respectively.The limits of quantitation were 1.782 1,2.079 0,0.749 8,1.777 8,0.223 1,0.607 0 μg/mL;the limits of detection were 0.594 0,0.693 0,0.249 9,0.592 6,0.074 4,0.202 3 μg/mL,respectively.RSD of precision test was lower than 2.0％.Only acetone and isopropyl alcohol were detected in stability test and reproducibility tests,RSD＜2.0％.Their recoveries were 99.34-100.75％ (RSD=0.52％,n=9),98.20％-100.24％ (RSD=0.69％,n=9),98.07％-100.07％ (RSD=0.84％,n=9),99.86％-101.32％ (RSD=0.58％,n=9),97.87％-104.02％ (RSD=2.13％,n=9),98.26 ％-100.58 ％ (RSD =0.75 ％,n =9),respectively.CONCLUSIONS:The established method is simple,accurate and reproducible,and can be used for simultaneous determination of 6 residual organic solvents in aprepitant raw material.
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OBJECTIVE:To establish a method for the determination of 1,1-ethanediol diacetate and acetic acid in flurbiprofen axetil. METHODS:Capillary gas chromatography was performed on the column of DB-FFAP capillary column by temperature pro-grammed,the inlet temperature was 150 ℃,flame ionization detector was chosen,detector temperature was 290 ℃,carrier gas was nitrogen at a flow rate of 1.0 ml/min,injection volume was 1.0 μl,and split ratio was 5∶1. RESULTS:1,1-ethanediol diacetate and acetic acid were well-separated;and the linear ranges was 0.78-19.55 g/ml(r=0.999 7)and 7.69-64.11 μg/ml(r=0.999 3),re-spectively;the limits of quantification were 0.78 μg/ml and 7.69 μg/ml,and limits of detection were 0.23 μg/ml and 2.56 μg/ml for 1,1-ethanediol diacetate and acetic acid respectively;RSDs of precision and reprocudibility tests were lower than 3%,and stability test was lower than 5%;recoveries were 97.6%-100.4%(RSD=0.94%,n=9)and 93.6%-100.4%(RSD=0.94%,n=9);and the test results for 3 batches of flurbiprofen axetil were met the specification. CONCLUSIONS:The method is simple,accurate and re-liable,and can be used for the determination of 1,1-ethanediol diacetate and acetic acid in flurbiprofen axetil.
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Objective To improve the quality of aiye processed products, an eucalyptol content in commercially available aiye two processed products of chao aiye and aiye tan was investigated.Methods A capillary gas chromatography was used.The sample was prepared with n-hexane by reflux condensation.Chromatographic conditions: The separation was carried on an Ailgent DB-1 capillary column(30 mm ×0.320 mm ×0.25 μm). Inlet temperature was 200℃ and FID temperature was 250℃.The programmed column temperature was set as follows:maintained at 100℃ for 6 min and raised to 160℃ at the rate of 20℃/min followed by holding for 3min.The splitting-ratio was 5.0:1.The carried gas was nitrogen, flow rate was 1.0 mL/min.Injection volume was 1μL.Results In the given chromatographic conditions, the eucalyptol chromatographic separation had good, and the separation degree was greater than 1.5 between eucalyptol and other impurity peak.The linear range of eucalyptol was 11.4-114.0 mg/mL(r=0.999 5). Methods repeatability and recovery were good.The minimum limit of quantification was 0.5μg/mL.The results of determination of eucalyptol show that the eucalyptol content in the commercially available 11 batch of chao aiye was between 5.6-78.2 μg /g, and 12 batch of aiye tan had no eucalyptol. Conclusion The processing technology of current commercially available aiye processed products of chao aiye and aiye tan need to be improved, and the quality standard need to be improved.
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This study was aimed to establish the determination method of nineorganic solvent residues of macrop-orous resin. Headspace capillary gas chromatography (GC) was used in the content determination of hexane, benzene, methyl-benzene, o-xylene, m-xylene, p-xylene, styrene, diethyl-benzene and divinyl-benzene of macroporousresin residues in Ginkgo leaf tablets. The results showed that ninemacroporous resin residues in Ginkgo leaf tablets were completely separated. The calibration curves were in good linearity (r=0.9992-0.9998). The average recoveries were 80%-110%. It was concluded that themethod was accurate, quick, and sensitive, which can be used to determine the macroporous resin residues in Ginkgo leaf tablets.
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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 capillary gas chromatography method for the determination of trinitrotoluene (TNT) in workplace air.Methods Using dichloromethane as the eluent,the air was drawn through a glass fiber filter to collect TNT,TNT was extracted from the filter with dichloromethane by an ultrasonic shaker,and the sample was analyzed by OV-17 elastic quartz electron capture detector capillary gas chromatography.Results Under the optimal condition,the lowest detection limit was 0.006 ?g/ml,the lowest detection concentration was 0.001 3 mg/m~3 (based on 45 L air sample).When the concentration of standard solution was 0.040-2.0 ?g/ml,the linear equation was good,r=0.999 8,RSDs were between 0.66%-3.62%,the recovery rates were 90.4%-95.5%.When sample was collected by fiberglass filter paper,the efficiency of desorption was more than 90%,and was stable for at least 7 days at 2℃-8℃.Conclusion This method is applicable to the determination of trinitrotoluene in workplace air.
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Objective To establish a capillary gas chromatography method for the determination of menthol and methyl salicylate in Shangtongning adhesive plaster. Methods The internal standard substance of n-Pentadecane was employed. The GC system consisted of a DB-WAX capillary column (30 m?0.32 mm, 0.25 ?m), nitrogen as the carrier gas, column temperature at 130 ℃, FID as the detector at 200 ℃, and with a split ratio of 12∶1. Results The contents of menthol and methyl salicylate in 6 lots of samples were determined and the constituents concerned were separated well under the chromatographic condition. The average recovery of menthol and methyl salicylate were 101.52% (RSD=2.66%) and 100.34% (RSD=3.38%), respectively. Conclusion The method was sensitive, accurate, specific and suitable for the quality control of the preparation.
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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.
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0.999 9).The minimum quantitative concentrations were 0.027 ?g?mL-1,0.033 ?g?mL-1,0.095 ?g?mL-1,respectively.The 3 kinds of organic solvents were not found in each batch except 0.10% and 0.15% ethyl acetate was found in 2 batches of samples.CONCLUSIONS:The established method is accurate,sensitive and accurate for the determination of 3 kinds of residual organic solvents in beclometasone dipropionate simultaneously.
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OBJECTIVE: To determine the residual levels of 4 organic solvents(methanol,alcohol,ether and acetone) in the raw material of medicinal sodium ozagrel by capillary gas(GC) chromatography.METHODS: The determination was performed using hydrogen flame ionization detector,AB-CarboWax with nitrogen gas as carrier gas using temperature programming for the column temperature.The sample size was 1 ?L,the temperature of the detector was 280 ℃,the temperature for sample injection was 250 ℃,the flow rate of carrier gas was 1 mL?min-1,and the flow rate of the hydrogen gas was 40 mL?min-1.RESULTS: The linear ranges of methanol was 0.037 5～3 mg?mL-1,alcohol,ether and acetone were 0.062 5～5 mg?mL-1,respectively,their average recoveries ranged from 98.07% to 99.12% with RSD being 0.34%～0.65%.Their lowest detection limits were all less than 3.125 ?g?mL-1,which were undetected for all the samples.CONCLUSIONS: The method is simple,sensitive and accurate,and it can be used for the determination of the residual levels of organic solvents in the raw medicinal of sodium ozagrel.
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Objective To develop a quality standard of Citrus limon oils.Methods Limonene in Citrus limon oils was identified by capillary gas chromatography and its content was determined by internal standard method.A polyethylene glycol elastic quartz capillary column (30 m of length,0.32 mm of internal diameter,0.25?m of film thickness) was used,column temperature being 90℃and split ratio being 5:1.Results In the range of 0.0627 mg/mL～4.0136 mg/mL for limonene,an equation was obtained:Y=1.53321X-0.05275,r=0.999 9.The average recovery of limonene was 97.2 % with RSD being 0.6 %.Conclusion The method is stable and reliable,and can provide evi- dences for the development of quality standard of Citrus limon oils.
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Objective: To determine magnolol and honokiol in Huoxiangzhengqi Capsule(oil of Herba Agastachis, oil of Perillae, Pericarpium Citri Reticulatae, Cortex Magnoliae Officinalis, etc.).Methods: A supercritical Fluid Extraction (SFE) has been used to extract magnolol and honokiol in Huoxiangzhengqi Capsule, and CGC was used to analyse the extracts.Results: The average rccovery was 96.81% ( RSD =2.81%, n =5) for magnolol, and 97.75% ( RSD =2.36%, n =5) for honokiol, respectively. Conclusion: The SFE CGC offline method for the analysis of Huoxiangzhengqi capsule is simple, quick and accurate.
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Objective: To establish a new method for determination of ? pinene in Folium Pini. Method: The contents of ? pinene were determined by high performance capillary gas chromatography with sequential increase of temperature programming. Results: The calibration curve showed good linearity over the range of 0.424 2.12?g( r =0.9999). The average recovery was 97.9% and the relative standard deviation was 2.9%( n =5), and it was found that the contents of ? pinene in dry herbs were markedly different from the contents in fresh herbs. Conclusion: The method is simple, and accurate with a good reproducibility and can be applied as quantitative analysis method for Folium Pini.
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AIM: To study the volatile oil of GanluXiaodu Granules GLXD (Talcum, Herba Artemisiae Scopariae, Radix Scutellariae etc.) and establish it's fingerprint. METHODS: By capillary gas chromatography. RESULTS: The fingerprints of volatile oil in Ganlu Xiaodu Granules were composed of 56 peaks, among which there were 17 characteristic peaks, having 86.97% of total area of the whole fingerprints peaks. The average RSD of retention time of characteristic peaks was 0.33%, that of peak-area was 2.76%. CONCLUSION: The fingerprints of volatile in Ganlu Xiaodu Granules can be used to control the quality.
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Objective To develop a method of determining benzene hydrocarbon and halogenated alkane hydrocarbon in the air of workplaces with the capillary gas chromatography of carbon disulphide desorption. Methods Benzene hydrocarbon and halogenated alkane hydrocarbon in the air of workplace were collected by active carbon sampling cuvette, then separated by hydrogen flames detector gas chromatography machine after carbon disulphide desorption. Benzene hydrocarbon and halogenated alkane hydrocarbon were determined quantitively by retention time and quantitatively by apex area. Results The linear ranges of benzene, toluene, p-xylene, m-xylene, o-xylene, ethyl benzene, styenl, chlorobenzene, acetone, carbontetrachloride, dichloromethanl, trichloromethane, 1, 2-dichloroethane, naphth alene were 0.019-81.600, 0.018-91.200, 0.018-88.800, 0.018-56.8, 0.011-92.000, 0.012-63.200, 0.018-93.200, 0.449-2298.400, 0.252-1287.000 and 0.076-390.000 mg/m3 respectively. The recovery rates were 88.4%-98.6% and RSD were 1.0%-6.0%. Conclusion This method can separate efficiently and determine accurately benzene hydrocarbon and halogenated alkane hydrocarbon in the air with a good precision. It is suitable for the determination of the toxicants in the air.
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Objective A method for the determination of 4-methylimidazole in soy sauce by capillary gas chromatography was studies.Methods The method consisted of a methylene chloride to elution,followed by concentration of the eluate.N,N-Dimethylaniline(IS) was added in and GC analysis of the eluate,prior to GC analysis.The GC analysis was carried out by DB-FFAP capillary column and nitrogen phosphorus detector(NPD).Results The linear range was 4.9mg~1.5?102 mg/L and the limit of detection was 0.16 ug/L.The average recoveries were 97.25%and 99.44% by stand addition method in 0.0102mg and 0.0602mg 4-methylimidazole.Conclusion The method was simple,rapid and sensitive.A useful method for determining 4-methylimidazole in soy sauce was provided for forensic analysis.
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A gas chromatographic method was established for the analysis of fatty acid composition of oils. After methlation of the samples, the retention time of the fatty acid esters in the glass capillary coated with crosslin-ked methyl silicone was closely related to the number of carbon atoms.The reproducibity of this method was satisfactory. The relative standard deviation was 0.4-1.5%. Six kinds of vegetable oils were analyzed by this method, and the results were consistent with those reported by Canadian Cereal Association. For analysis of the free fatty acid composition of becte-ria, the results were comparable with those obtained from thin layer chroma-tography and chemical analysis.