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Objective:To optimize the processing technology of Moslae Herba processed with ginger juice, and to explore the changes of its volatile components in processing process. Method:The volatile components in Moslae Herba, ginger juice and Moslae Herba processed with ginger juice were extracted by steam distillation. Volatile components in these products were analyzed by HS-GC-MS and identified by NIST 11 standard mass spectra library. Gas chromatographic conditions were as following:HP-5MS elastic quartz capillary column(0.25 mm×30 m, 0.25 μm), helium as the carrier gas, flow rate of 1.0 mL·min-1, injector temperature at 250℃, sample quantity of 0.2 μL, split ratio of 50:1, temperature program for initial temperature at 40℃, up to 60℃ with the heating rate at 5℃·min-1, keep 2 min, up to 160℃ with the heating rate at 5℃·min-1, keep 3 min, finally rise to 250℃ with the heating rate at 25℃·min-1, keep it for 2 min and finish, mass spectrometry conditions were as following:electron impact ionization(EI), electron collision energy of 70 eV, ion source temperature at 230℃, the interface temperature at 280℃, quadrupole temperature at 150℃, no delay of solvent, electronic multiplier voltage at 2.188 kV, taking full scan mode, scanning range of m/z 35-550.Taking frying time, solid-liquid ratio and moistening time as factors, orthogonal test was adopted to optimize the processing technology with the comprehensive score of relative contents of thymol and carvacrol, number of volatile components and extracting amount of volatile oil as index. Result:A total of 27 volatile components were detected in Moslae Herba. There were 81 volatile components in Zingiberis Rhizoma Recens. The processed products of orthogonal test(No. 1-9) had 31, 38, 29, 35, 38, 33, 34, 22 and 26 volatile components, respectively. Extracting amount of volatile oil was in the order of Moslae Herba processed with ginger juice > Zingiberis Rhizoma Recens > Moslae Herba. The best processing technology was as following:moistening Moslae Herba with equal volume of ginger juice for 6 h, stir-frying for 8 min. Conclusion:Processing has certain impact on the extracting amount of volatile oil in Moslae Herba and the types of volatile components. This optimized technology is stable and feasible, which can provide experimental data for the quality evaluation of processed products of Moslae Herba, and lay a foundation for clarifying its processing mechanism.
RESUMO
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 .
RESUMO
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.
RESUMO
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.