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Objective:To understand the basic situation of visible particles in Shengmai injection,and study the visible particles control and inspection for Shengmai injection. Methods: The samples of Shengmai injection were collected and the visible particles were checked by light inspection and light scattering,and the results were summarized and analyzed. The exogenous factors and endog-enous factors affecting the visible particles in Shengmai injection were investigated. Results:The positive inspection rate of visible par-ticles in Shengmai injection in market was low. Light,temperature and pH value had mild influence on the visible particles in Sheng-mai injection. Conclusion:The control measurement for the visible particles in Shengmai injection in every enterprise is effective,and the quality control is promising.
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Objective:To improve the quality standard for Anweiyang capsules. Methods: TLC was used to identify Glycyrrhiza inflata Bat. Licochalcone A was determined by RP-HPLC. Using a C18 Column, the mobile phase consisted of acetonitrile-0. 1% phos-phoric acid(40:60), and the detection wavelength was at 376 nm. Results:The herb could be identified by TLC. For licochalcone A, the linear range was from 25. 563 to 1 533. 798 ng, and the average recovery was 99. 8%(n=9). Conclusion:The method is simple and accurate, which can be used to improve and control the quality of Anweiyang capsules.
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Objective:To develop a method for determining deoxynivalenol in four kinds of traditional Chinese herbal medicines. Methods:After being extracted by water, purified by an immunoaffinity column, deoxynivalenol was analyzed by LC-MS-MS. Results:The calibration curve was linear within the range of 2-50 ng·ml-1 for deoxynivalenol. The recovery was 68. 7%-88. 3%. Conclusion:The method is simple, sensitive and accurate in the determination of deoxynivalenol in Semen Ziziphi Spinosae, Semen Sojae Praepara-tum, Semen Coicis and Fructus Psoraleae.
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This paper aims to establish a method for the determination of sulfur dioxide in sulfur fumigation Chinese herbs. Sample powder and hydrochloric acid solution were isolated by paraffin layer in order to avoid early reactions, with the generation of sulfur dioxide, headspace with airtight needle was used to transfer sulfur dioxide into gas chromatograph, and detected with thermal conductivity detector. The analytical performance was demonstrated by the analysis of 12 herbs, spiked at four concentration levels. In general, the recoveries ranging from 70% to 110%, with relative standard deviations (RSDs) within 15%, were obtained. The limit of detection (LOD) was below 10 mg x kg(-1). Standard addition can be used for low recovery samples. The method is simple, less time-consuming, specific and sensitive. Methods comparison revealed that gas chromatography is better than traditional titration in terms of method operability, accuracy and specificity, showing good application value.
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A method of LC-QTOF/MS combining with chemical synthesis has been used to determine the structures of three novel bile acids from bear bile powder. Reference substances of tauroursodeoxycholic acid and taurochenodeoxycholic acid were oxidized by pyridinium chlorochromate. The products were analyzed by LC-QTOF/MS. Total 4 products including 3 isomers were predicted and identified according to the PCC oxidation theory and LC-QTOF/MS results. Bear bile powder samples were dissolved by methanol and analyzed by LC-QTOF/MS. Three unknown peaks were found and identified as 2-[[(3beta, 5beta)-3-hydroxy-7, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, 2-[[(5beta)-3, 7, 24-trioxocholan-24-yl]amino]-ethanesulfonic acid and 2-[[(5beta, 7beta)-7-hydroxy-3, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, separately, by matching their results with that of oxidation products above.
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AIM:To study a method for the determination of 13 N-methylcarbamate peticides in traditional Chinese herbal medicines(TCHMs).METHODS:Thirteen pesticides were extracted by acetonitrile,and purified through solid phase extraction(SPE)cartridges,then detected by HPLC with post-column derivatization and Fluorescense Detector excited wavelength was 330 nm,emissive wavelength was 465 nm.RESULTS:The analytical performance was demonstrated by the analysis of 6 TCHMs samples' extracts,spiked at three concentration levels for each pesticide.In general,the recoveries ranging from 74.1 to 108.8%,with relative standard deviations(RSDs)better than 15%,were obtained.The limit of quantification(LOD)of 13 pesticides from 0.000 3 to 0.06 mg/kg.CONCLUSION:The method has good extraction efficiency and purification effect,which could be standard of N-methylcarbamate peticides residues in the routine analysis of TCMs.
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AIM: The multi-residues method was used to determine organophosphorus pesticides in traditional Chinese herbal medicines (TCHMs).METHODS: Fifty three pesticides were extracted by high-speed homogenization,and then cleaned sequentially by C_(18) and Carb/NH2 solid phase extraction (SPE) cartridges.The residues were simultaneously identified and quantified by GC-FPD equipped with dual tower,dual column and two FPD detectors.RESULTS: The analytical performance was demonstrated by the analysis of 6 TCHMs samples extracts,spiked at three concentration levels for each pesticide.In general,the recoveries ranging from 70% to 120%,with relative standard deviations (RSDs) less than 15%,were obtained.The limit of detection (LOD) for most of the targeted pesticides tested was below 0.01 mg/kg.CONCLUSION: The method has good extraction efficiency,purification effect and good reproducibility,which can be applied to the determination of organophosphorus pesticide residues in the routine analysis of TCHMs.
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The paper is to report the establishment of a method for the determination of multi-residue organochlorine and pyrethroid pesticides in traditional Chinese medicines (TCMs). Fifty-six pesticides were extracted by high-speed homogenization, and then purified through gel permeation chromatography (GPC) and solid phase extraction (SPE) cartridges. The residues were simultaneously identified and quantified by GC-ECD equipped with dual tower, dual column and two micro-ECD detectors. The analytical performance was demonstrated by the analysis of 3 TCMs samples' extracts, spiked at three concentration levels for each pesticide. In general, the recoveries ranging from 70% to 110%, with relative standard deviations (RSDs) better than 15%, were obtained. The limit of detection (LOD) for most of the targeted pesticides tested was below 0.01 mg kg(-1). The method had good extraction efficiency, purification effect and good reproducibility, which could be applied to the determination of organochlorine and pyrethroid pesticide residues in the routine analysis of TCMs.
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AIM:To establish the quality specification of Yinzhihuang Injection (extract of Herba Artemisiae scopariae,extract of Fructus Gardeniae,extract of Radix Scutellariae,extract of Flos Lonicerae Japonicae); METHODS:Extractum Artemisiae Scopariae、 Extractum Fructus gardeniae、 Extractum Flos lonicerae and Extractum Radix scutellariae were identified by TLC and were determined by HPLC. RESULTS:The average recoveries of chlorogenil、gardenoside、baicalin and p-hydroxyacetophenone were 99.8%,99.2%,100.1% and 99.9%,respectively.RSD were 0.81%,1.20%,1.90% and 0.55%,respectively.The TLC sports developed were fairly clear,and the blank test showed no interference. CONCLUSION:The method developed is simple and accurate with good reproducibility,and the method can be used for quality control of Yinzhihuang Injection.
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AIM: To establish the GC method for the determination of linalool of Rhizoma Homalomenae. METHODS:The column consisted of Fused Silica Capillary Polyethylene Glyol(30 m?0.25 mm?0.25 ?m),column temperature was at 120 ℃,Injection port temperature at 260 ℃,Detector temperature at 300 ℃,flow rate was 1.0 ml/min. RESULTS: Linalool has a good linearity in the range of 0.011 985～1.997 5 ?g.The recovery rate was 99.2%,RSD was 1.63%. CONCLUSION: The method developed is simple and accurate with good reproducibility,and can be used for quality control of Rhizoma Homalomenae.
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AIM: To establish the quality standard of Wumeirendan (Fructus Mume, Radix et Rhizoma Glycyrrhizae, Mentholm, etc.) METHODS: Fructus Mume was identified by TLC. Menthol was determined by GC, Ammonium glycyrrhiziate was determined by HPLC. RESULTS: The average recoveries were 103.5% and 100.3%, RSD were 0.76% and 1.03%. The TLC sports developed were fairly clear, and the blank test showed no interference. CONCLUSION:The method developed is simple and accurate with good reproducibility, and the method can be used for quality control of Wumeirendan.
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AIM: To establish the quality standard of Yupingfeng Oral Liquid(Radix Astragali,Radix Sapo-shnikoviae,Rhizoma Atractylodis Macrocephalae,etc.); METHODS:Rhizoma atractylodis macrocephalae was (identified) by TLC,Radix Saposhnikoviae was identified by HPLC;astrayloside Ⅳ was determined by HPLC.( RESULTS):The recovery of astragloside Ⅳ was 96.7%,RSD was 1.74%.The TLC sports developed were fairly clear,and the blank test showed no interference. CONCLUSION:The mothod developed is simple and accurate with good reproducibility,and the mothod can be used for quality control of Yupingfeng Oral Liquid. withgood