ABSTRACT
OBJECTIVE: To establish a method for determination of astragaloside in 4 Chinese patent medicines (BuZhong YiQi Pills, TongQiao BiYan Granules, XingNao ZaiZao Capsules, YuPing Feng Granules) by accelerate solvent extraction (ASE) combined with column post compensation liquid chromatography and charged aerosol detector (CAD) detection, and compare the result with that of the pharmacopoeia method. METHODS: The optimal extraction conditions were determined by the ASE test: water saturated n-butanol was used as solvent, ASE extraction temperature was 100℃, extraction time was 7 min and cycle time was 3. For the HPLC analysis, Thermo AQ-C18 column (2.1 mm × 100 mm, 3 μm) was employed, the mobile phase for the analysis pump was composed of acetonitrile-water (15:85), and the flow rate was 0.3 mL•min-1. Gradient program was as follows: 0 min, 15% A; 0 - 4 min, 15% - 60%A; 4 - 5 min 60% A. The mobile phase for the compensating pump was acetonitrile, and the flow rate was 0.3 mL•min-1. RESULTS: The linear range of the calibration curve of astragaloside was 26.62 - 665.5 μg•mL-1. The RSD of sample analysis was 1.0% - 2.1%. The average recoveries were 98.80% - 100.80%. The method is in good agreement with the Pharmacopoeia method. CONCLUSION: The method is rapid, accurate and reproducible. It can be used for the determination of astragaloside in 4 kinds of Chinese patent medicines.
ABSTRACT
Objective: To establish an accelerated solvent extraction(ASE)-HPLC method to determine chrysophanol and aurantio-obtusin in Cassia obtusifolia L.Methods: The optimal extraction conditions were defined by orthogonal tests using ASE.The method was carried out on an ACE Excel C18-PFP column (75 mm×2.1 mm,2.5 μm) with the mobile phase consisting of 0.1% phosphoric acid solution-acetonitrile with gradient elution.The column temperature was 40 ℃,the flow rate was 0.4 ml·min-1, and the detection wavelength was 284 nm. Results: The best process parameters of ASE were as follows:the extraction solvent was methanol, the extraction temperature was 120 ℃ and the static extraction duration was 5 minutes for three cycles.The ASE method needed only 1/9 of the time as the pharmacopoeia method,while the extraction efficiency of the ASE method was higher.The linear ranges of cassia obtusifolia L.and Chrysophanol were at 0.73~58.57 μg·ml-1(r=0.999 7) and 1.09~87.29 μg·ml-1(r=0.999 6).The average recoveries were 102.7%(RSD=0.8%) and 98.2%(RSD=1.5%).Conclusion: The method is simple, rapid and sensitive, which can be used for the rapid determination of aurantio obtusin and chrysophanol in Cassia obtusifolia L.
ABSTRACT
A method for determination of 16 kinds of polycyclic aromatic hydrocarbons ( PAHs ) in atmospheric fine particles ( PM2. 5) was developed based on accelerated solvent extraction-direct injection coupled with high performance liquid chromatography (HPLC). PM2. 5 was collected by glass fiber membrane filter and pretreated with acetonitrile by accelerated solvent extraction. The extract was separated by ZORBAX Eclipse PAH column with acetonitrile and water as mobile phase, and detected by ultraviolet and fluorescence detectors. The result showed that the 16 kinds of PAHs were well separated and there were good linear relationships ( r≥0. 9998) in the concentration range of 0. 025 -5. 00 μg / mL. The recoveries were from 78. 3% to 113. 2% . The relative standard deviations ranged from 0. 5% to 9. 5% . The detection limits were 0. 007 - 0. 062 ng / m3 . The method was simple, rapid, accurate and sensitive, and suitable for the simultaneous determination of 16 kinds of PAHS in PM2. 5.
ABSTRACT
Objective: To establish an accelerated solvent extraction (ASE)-charged aerosol detector (CAD) method for simultaneous detection of jujuboside A, jujuboside B, spinosin, and betulinic acid in Zizyphi Spinosae Semen. Methods: The orthogonal design was applied to optimize the extraction parameters of the ASE system. The target compounds were detected by HPLC-CAD with the parameters as follow: Thermo Syncronis C18 (100 mm × 3 mm, 3 μm) column, a gradient elution program with acetonitrile-water as mobile phase at a flow rate of 0.5 mL/min, the column temperature was kept at 40℃. Detector was Corona Ultra CAD with 35℃ of nebulization temperature. Results: Optimization of the ASE parameters with orthogonal design greatly improved the extraction efficiency; All the target compounds could be simultaneously determined in a single run. Good linear relationships (0.998 3-0.999 6) and high relative recoveries were 98.46%-102.02%. Conclusion: The method is rapid, simple, accurate, and thus could be used for the quality control of Zizyphi Spinosae Semen.
ABSTRACT
Objective: To establish a method of rapid analysis for simultaneous determination of oleanolic acid and ursolic acid in Chinese materia medica (CMM) of Verbena officinalis, Ligustrum lucidum, Prunella vulgaris, Hedyotis diffusa, Patrinia scabiosaefolia, Eriobotrya japonica, Crataegus pinnatifida, Chaenomeles Fructus papaya. Methods: The analyses of preparation were conducted by accelerated solvent extraction (ASE), methanol was used as solvent extraction, and the static extraction time was 6 min. Separation was carried out on Acclaim C30 Thermo column with acetonitrile and 0.2% acetic acid (85:15) as mobile phase, flow rate was 0.3 mL/min, and UV detection wavelength was set at 205 nm. Results: After 10 min sample extraction time, oleanolic acid and ursolic acid reached baseline separation, and no sample matrix was interfered, the linear correlation coefficient was over 0.999, the average recovery between 95.8% and 102.7%; Compared to Chinese Pharmacopoeia 2015, the determination of average mass fraction difference was 3.7% and 5.8%. Conclusion: This method is simple, fast, and suitable for the analysis of these drugs, and it can be used for content determination of oleanolic acid and ursolic acid for eight kinds of CMM.
ABSTRACT
OBJECTIVE:To establish the method for simultaneous determination of 9 common inorganic anions in Huanglian shangqing tablet. METHODS:The accelerated solvent extraction-ion chromatography was adopted. Inorganic anions were deter-mined by Ion Pac AS11-HC anion exchange column,protected by Ion Pac AG11-HC column and eluted by hydroxide potassium so-lution(gradient elution)at the flow rate of 1.2 mL/min. The column temperature was set at 30 ℃,elution time was 18 min,and sample volume was 25 mL. RESULTS:The linear ranges of fluorinion,formate ion,nitrite ion,bromide ion,nitrate ion,sulfate ion,oxalate ion and phosphate ion were 0.1-5 mg/L(r=0.9990-0.9999). The limits of quantitation were 0.020,0.078,0.030, 0.058,0.052,0.068,0.084,0.064,0.074 mg/L,and the limits of detection were 0.005,0.024,0.008,0.017,0.015,0.022, 0.026,0.020,0.021 mg/L,respectively. RSDs of precision,stability and repeatability were all lower than 4.0%;recoveries were 80.00%-125.08%(RSD ranged 0.97%-2.47%). CONCLUSIONS:The method is simple,precise,stable and repeatable,and can be used for 9 common inorganic anions in Huanglian shangqing tablet.
ABSTRACT
Waste printed circuit boards(W-PCBs) were multiple smashed and separated, then passed through a 60-mesh screen, treated with hydrochloric acid (2 mol/L), ultrapure water and dehydrated with acetone successively.The filter residue and filter paper were filled into the extraction pool, or inserted into Soxhlet Extraction tube parceled with new filter paper.After addition of 5 μL of internal standard substance, the filter residue above was respectively extracted by Soxhlet Extraction (SE) method or Accelerated Solvent Extraction (ASE) method, cleaned with multi-layer silica gel column and activated-charcoal column to obtained the dioxins samples.The samples were analyzed by isotope dilution high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS).The effects of SE and ASE method and number of chlorines atoms on recovery of 15 kinds of 13C-2,3,7,8 PCDD/Fs were investigated, and the accuracy and precision of the two extraction methods were compared.The results show that, the recovery of 15 kinds of 13C-2,3,7,8 PCDD/Fs using ASE method is 54.3%-113.0%, and that of SE is 28.3%-77.7%, and the Toxic Equivalent Quangtity (TEQ) in W-PCBs is 0.075 ng/kg (TEQ) and 0.266 ng/kg (TEQ) using ASE and SE method respectively.Under the premise that accuracy and precision meet with the international standard, ASE is simple, rapid, solvent-free and accurate.
ABSTRACT
Objective:To study the feasibility of the determination of ephedrine hydrochloride in Tongxuan Lifei pills by acceler-ated solvent extraction ( ASE) combined with QuEChERS purification, and compare the results with those of the extraction method in Chinese Pharmacopoeia. Methods: The extraction efficiency of ephedrine hydrochloride in Tongxuan Lifei pills determined by HPLC was used as the evaluation index, and the operation parameters of ASE were optimized by orthogonal experiments. Results: The opti-mum conditions of ASE for the determination of ephedrine hydrochloride in Tongxuan Lifei pills were as follows:the samples were defat-ted by n-hexane ( the extraction temperature was 80℃, the static extraction time was 5 min for one cycle, and the flush volume was 100%. ) ,and then methanol was used as the extraction solvent for the extraction of ephedrine hydrochloride ( the extraction temperature was 80℃,the static extraction time was 8 min for three cycles) ,in the end, the impurities were purified by PSA purifying agent. Using the optimized ASE method to extract ephedrine hydrochloride in Tongxuan Lifei pills, the extraction time was reduced to 40 minutes with less interference, and compared with that of the method in Chinese Pharmacopoeia, the determination of the relative standard devi-ation was less than 5%. Conclusion:The ASE technique combined with QuEChERS purification is simple, quick and effective,and it can be used as the pretreatment method for the determination of ephedrine hydrochloride in Tongxuan Lifei pills.
ABSTRACT
OBJECTIVE:To develop a new way for the extration and determination of naringin in Davallia mariesii. METH-ODS:Naringin in D. mariesii was extracted by ASE350 accelerated solvent extraction system;HPLC was performed for the con-tent determination of naringin in D. mariesii,the column was Kinetex XB-C18 with mobile phase of methanol-5%acetic acid(25∶75, V/V)at a flow rate of 0.8 ml/min,detection wavelength was 283 nm,column temperature was 40℃,and injection volume was 10 μl. RESULTS:The linear range of naringin was 0.073 0-0.730 0 μg(r=0.999 9);the limit of quantitation was 0.73 μg,the limit of detection was 0.022 μ g;RSDs of precision, stability and reproducibility tests were lower than 2% ;recovery was 98.92%-100.85%(RSD=0.72%,n=6). CONCLUSIONS:The method is simple,accurate and specific,and can be used for the content determination of naringin in D. Mariesii.
ABSTRACT
A sensitive and convenient method based on accelerated solvent extraction ( ASE )-liquid chromatography tandem mass spectrometry (LC-MS / MS) was established for the simultaneous determination of 11 phthalic acid esters(PAEs) in soil. The optimized conditions were as follows: By using n-hexane as the extraction solvent, spiked sample was extracted by ASE at 160 ℃ for 4 times, 12 min for each time. The extract was concentrated by evaporation. Qualitative and quantitative analysis was carried out by the multiple reaction monitoring mode after the chromatographic separation with atmospheric pressure chemical ionization (APCI), using acetonitrile -0. 1% formic acid water as mobile phase. The limits of detection(LODs) for 11 PAEs were between 0. 03 - 13. 0 μg / kg. The recoveries and relative standard deviations were 72. 8% -101. 8% and 1. 7-6. 7% , respectively. This method is rapid, sensitive and suitable for the determination of PAEs in soil.
ABSTRACT
A novel HPLC-CAD method coupled with on-line solid phase extraction ( SPE ) for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite, 5. 0 g manure sample was put into the cell and extracted with hot water at 70℃ and 10. 3 MPa. An on-line SPE methodology was applied to pre-treat the sample, and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0. 1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6. 3 μg/kg. The average recoveries were 79. 2%-87. 5%.
ABSTRACT
Soil water is one of the most important components in hydrological cycle. The stable hydrogen and oxygen isotopes in soil water have been increasingly used in the ecological, environment and hydrological research. In view of different techniques for extracting soil water, there is significant difference in theδD andδ18 O composition. This paper presents a method for analyzing hydrogen and oxygen isotopes in soil water by using elemental analyzer and isotope ratio mass spectrometry with accelerated solvent extraction for sample pretreatment. The conditions are: extraction solvent: dichloromethane, temperature: 100 ℃, pressure of 10. 3 MPa, static time:10 min. The samples were extracted three times, and with cycle values of four, four and three, respectively. Comparing with the added water, the deuterium and oxygen isotope values in the extracted soil water enrich 2. 12‰-4. 58‰ and 0. 17‰-0. 93‰, respectively. The reproducibility of replicate extractions of soil water is around ±0. 89‰ for δD and ±0. 37‰ for δ18 O.
ABSTRACT
Objective To compare the effects of accelerated solvent extraction (ASE), ultrasonic extraction (USE) and soxhlet extraction (SE), by extraction and determination of pesticide residues in Chinese herbal medicines. Methods Pesticide residues of Chinese herbal medicines were extracted by accelerated solvent extraction, ultrasonic extraction and soxhlet extraction, then the extract were cleaned up by sulfonation treatment, alumina neutral-florisil column and gel permeation chromatography (GPC). The extract was separated by HP-5 capillary column and detected by electron-capture detector. Results Extraction efficiency of USE was significantly lower than that of ASE and SE, there was no significant difference between ASE and SE. Pairwise comparison of the recoveries of three purification methods showed no significant difference. Conclusion The extraction efficiency of three methods was ASE>SE>USE. The extraction method should be selected according to the requirement.
ABSTRACT
Objective To develop the accelerated solvent extraction (ASE ) for determ ining pesticides pre-sent in blood sam ples. Methods Pesticides were extracted by ASE with optimized param eters to study recovery rate affected by extraction tem perature, time and agent. GC/MS was used to perform quantita-tive analysis.Results The recovery rates of eight pesticides were 70.6%-92.4%. The coefficient of variation was less than 5.0%. Agood linear relationship was obtained at the concentration range of 0.5-5.0μg/m L . Conclusion The m ethod was fast and sim ple with high recovery rate and good repeatability. It can be applied to analyze pesticides present in the blood specimen.
ABSTRACT
Objective: To develop a new method based on hydrophilic interaction chromatography-electrospray ionization-time of flight-mass spectrometry (HILIC-DAD-ESI-TOF/MS) for the rapid identification of the active components in Syngnathus acus and the development of their specific fingerprint chromatograms. Methods: Samples were extracted by accelerated solvent extraction, and the extraction conditions were optimized. The developed HILIC-DAD-ESI-TOF/MS method was used to identify the components in water extract from S. acus, and a chromatographic fingerprint based on HILIC analysis was established. Results: Ten compounds in S. acus extract could be primarily identified by HILIC-DAD-ESI-TOF/MS on-line detection, in which seven nucleosides were determined. The HPLC characteristic fingerprint was established on the basis of analysis on the multi batches of S. acus, which could be used to evaluate the quality of S. acus combined with similarity calculation. Conclusion: This method is simple and rapid, and is a powerful tool for the identification of S. acus.
ABSTRACT
Piperine and piperlongumine, alkaloids having diverse biological activities, commonly occur in roots of Piper longum L., Piperaceae, which have high commercial, economical and medicinal value. In present study, rapid, validated HPTLC method has been established for the determination of piperine and piperlongumine in methanolic root extract and its commercial formulation 'Mahasudarshan churna®' using ICH guidelines. The use of Accelerated Solvent Extraction (ASE) as an alternative to conventional techniques has been explored. The methanol extracts of root, its formulation and both standard solutions were applied on silica gel F254 HPTLC plates. The plates were developed in Twin chamber using mobile phase toluene: ethyl acetate (6:4, v/v) and scanned at 342 and 325 nm (λmax of piperine and piperlongumine, respectively) using Camag TLC scanner 3 with CATS 4 software. A linear relationship was obtained between response (peak area) and amount of piperine and piperlongumine in the range of 20-100 and 30-150 ng/spot, respectively; the correlation coefficient was 0.9957 and 0.9941 respectively. Sharp, symmetrical and well resolved peaks of piperine and piperlongumine spots resolved at Rf 0.51 and 0.74, respectively from other components of the sample extracts. The HPTLC method showed good linearity, recovery and high precision of both markers. Extraction of plant using ASE and rapid HPTLC method provides a new and powerful approach to estimate piperine and piperlongumine as phytomarkers in the extract as well as its commercial formulations for routine quality control.
ABSTRACT
OBJECTIVE: To study the optimal extraction technology of matrine and oxymatrine from Radix Sophorae Tonkinensis. METHODS: The total content of matrine and oxymatrine as the inspection index was determined using high performance liquid chromatography (HPLC). The extraction efficiency of warm immersion extraction, ultrasonic extraction, reflux extraction and accelerated solvent extraction (ASE) was compared. RESULTS: Accelerated solvent extraction was superior to the other three methods. The extraction conditions of accelerated solvent extraction were optimized through single-factor test and orthogonal experimental design. The sequence of influential significance was as follows: extraction times > ethanol concentration > extraction temperature > extraction time. The optimal technology of accelerated solvent extraction was that the ethanol concentration was 40%, extraction temperature was 90°C, the time of extraction was 13 min and the times of extraction was twice. The total content of matrine and oxymatrine from Radix sophorae tonkinensis was (15.5277 ± 0.4316) mg · g-1. CONCLUSION: The experiment has optimized the extraction method and parameters of alkaloid from Radix sophorae tonkinensis, which provides a new method for the extraction of alkaloid from Radix sophorae tonkinensis. Copyright 2012 by the Chinese Pharmaceutical Association.
ABSTRACT
Objective To introduce an accelerated solvent extraction (ASE) -HPLC-TOF/MS method for simultaneous determination of Polyphyllin I, Polyphyllin II, Polyphyllin VI, Polyphyllin VII, Dioscin and Gracillin in Paris Polyphylla. Methods The extraction was performed by ASE under the following conditions: extracting solvent 70% ethanol; extracting temperature 120°C; pressure 1. 17 MPa (1 700 psi); and static time 6 min. The separation was carried out on a MGC18 column (3.0 mm× 100 mm, 3. 0 μm). Elution was done with a linear gradient mobile phase system consisting of 0. 1% formic acid (V/V) water and acetonitrile. The flow rate was set at 0. 8 ml/min, the sample injection volume was 3 μl, the column temperature was kept constant at 25°C, nebulizer gas pressure was 275. 8 kPa (40 psi), drying gas flow rate was 10 L/min, and gas temperature was 350°C. Results The calibration curves for Polyphyllin I, Polyphyllin II, Polyphyllin VI, Polyphyllin VII, Dioscin and Gracillin were linear within the range of 0. 500 0-50. 00 μg/ml (r = 0. 999 8), 0. 422 3-42. 23 μg/ml (r = 0. 999 7), 0. 612 0-61. 20 μg/ml (r = 0. 999 9), 0. 714 0-71. 40 μg/ml (r = 0. 999 5), 0. 448 0-44. 80 μg/ml (r = 0. 999 9) and 0. 436 0-43.60 μg/ml (r = 0. 9997), respectively; and the average recoveries (n=6) were 98. 9%, 98. 0%, 102. 5%, 101. 9%, 103. 1% and 97. 9%, respectively. Conclusion The introduced method is solvent-saving and time-saving; it can also be used for high-throughput analysis and determination of steroidal saponins in Paris Polyphylla.
ABSTRACT
A comprehensive analytical method based on liquid chromatography tandem mass spectrometry has been developed for the determination of nonylphenol, octylphenol and bisphenol A in textiles and food packaging) materials. Various textile and food packaging material samples were extracted under the conditions of 10.3 MPa and 120 ℃ by accelerated solvent extraction method with two static cycles using ethanol as the extraction) solvent. The extract was cleaned up by Supelclean Envi-Carb solid phase extraction cartridge. Qualitative) and quantitative analyses were carried out for the analytes under the multiple reaction monitoring(MRM) mode after the chromatographic separation on Waters XBridge C_(18))(150 mm×2.1 mm, 3.5 μm) column) with methanol-0.1% NH_4OH gradient elution. The limits of detection(LODs) for alkylphenol, octyphenol and bisphenol A were 0.5 μg/kg. The mean recoveries for textile samples at the spiked level of 0.5-10 μg/kg were 86.9%-92.5%, with the relative standard deviation less than 9.1%. The mean recoveries for food packaging material samples at the spiked level of 0.5-10 μg/kg were 87.8%-93.0%, with the relative standard deviation less than 8.8%. The method is accurate, simple, rapid, and adapts to the inspection of nonylphenol, octylphenol and bisphenol A in textiles and food packaging materials.
ABSTRACT
An analytical method based on high performance liquid chromatography tandem mass spectrometry has been developed for the determination of 11 appetite suppressants (fenfluramine,phenylpropanolamine,sibutramine,sertraline,rimonabant,bupropion,citalopram,fluoxetine,benfluorex,topiramate,zoni-samide). Various weight-loss functional foods were extracted under accelerated solvent extraction and separated on Waters Atlantis T3( 150 mm×2.1 mm,3μm) column. The analysis was carried out on HPLC-MS/MS by electrospray ionization using multiple reaction monitoring. Identification was achieved by ihe retention time and the ion ratio,quantification was done by the external standard curves. The limits of detection for the appetite suppressants were 0.05-4.0 mg/kg. The mean recoveries at the three spiked levels(low,middle,high) were 78.3% - 103. 6% ,with the intra-day precision less than 12% and the inter-day precision less than 15%. The method is reliable,sensitive,reproducible,and adapts to the determination of the appetite suppressants in different weight-loss functional foods.