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Objective To establish a rapid and nondestructive method for the determination of multi-components in Salvia miltiorrhiza to improve the quality control of S. miltiorrhiza based on Near infrared spectroscopy combined with partial least squares (PLS) method. Methods A total of 106 batches of S. miltiorrhiza samples from different origins were collected. The content of 11 components (tanshinol sodium, protocatechuic aldehyde, caffeic acid, rosmarinic acid, alkannic acid, salvianolic acid B, salvianolic acid A, dihydrotanshinone, tanshinone I, cryptotanshinone, and tanshinone IIA) in all of the samples which was conducted as the reference value were determined by a UPLC method established in the previous research. And the NIRS spectrum were obtained under the integrating sphere diffuse reflection mode. The different processes of modeling were optimized by partial least squares (PLS) and other chemometrics methods, including the selection of calibration set and validation set, different pretreatment method, different spectral section, and the determination of factors. A linear quantitative calibration model between the near infrared spectrum and the content of the components to be measured was tried to be established so that the content of the components could be measured by NIRS rapidly. Results The predicted value of NIRS and the measured value of UPLC of five components in S. miltiorrhiza, including salvianolic acid B, dihydrotanshinone, tanshinone I, cryptotanshinone, and tanshinone IIA, presented a good linearity, indicating the calibration models had a preferable forecast results. The correlation coefficient were 0.981 1, 0.936 3, 0.960 5, 0.910 9, 0.978 0 respectively, and the mean and square deviation of the prediction set (RMSEP) were 0.957 0, 0.037 7, 0.041 6, 0.114, 0.063 9, respectively; But the model of the other constituents failed to reach the quantitative level. Conclusion The content of salvianolic acid B, dihydrotanshinone, tanshinone I, cryptotanshinone, tanshinone IIA in S. miltiorrhiza can be determined rapidly and nondestructive by the NIRS combined with PLS method, which lays a foundation for the rapid and field determination method for the medicinal materials and decoction pieces of S. miltiorrhiza.
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The aim of this study is to analyze the compositions of main bile acids in fermented and mixed processing products of arisame cum bile from pig bile, and to establish a method for content determination of bile acids in fermented Arisaema Cum Bile. Fermented and mixed processing products were prepared from arisaematis rhizome and arisaematis rhizoma preparatum with pig bile respectively. Then the differences in bile acids compositions between such two kinds of products were compared by high performance liquid chromatography and evaporative light-scattering detector (HPLC-ELSD). With three kinds of free bile acid compositions as the indicators, HPLC-ELSD method was adopted to determine the content of bile acid compositions in fermented product,on Agilent Eclipse XDB C₁₈(4.6 mm×250 mm, 5 μm) chromatographic column, with acetonitrile and 0.1% glacial acetic acid solution (55:45) as mobile phase, at a flow rate of 1 mL·min⁻¹, column temperature of 30 °C, drift tube temperature of 90 °C, and a nitrogen flow rate of 2.2 mL·min⁻¹. The results showed that the bile acids in fermented bile Arisaema were mainly in a free form, while in mixed processing product, the compositions were mainly in a conjugated form. Three kinds of free bile acids, namely porcine cholic acid (HCA), porcine deoxycholic acid (HDCA) and chenodeoxycholic acid (CDCA) in fermented product, showed a good linear relationship in the range of quantification. The average recovery rate was 95.99%-104.3%, complying with the requirements. The results showed that the conjugated bile acids could be transformed into free bile acids during the fermentation of arisaema cum bile. This established method can effectively control the content of bile acids compositions in fermenting arisaema cum bile.
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Animals , Arisaema , Bile , Bile Acids and Salts , Chromatography, High Pressure Liquid , Fermentation , SwineABSTRACT
Objective To improve the quality control standard of lidocaine hydrochloride injection .Methods A method for determination of related substances in lidocaine hydrochloride injection was established .Lidocaine hydrochloride was as‐sayed by HPLC .The chromatographic conditions :C18 chromatographic column was used .The mobile phase was phosphate buffer and acetonitrile (50∶50 ,adjusted to pH 8 with phosphoric acid) .The detection wavelength was 254 nm .Results Ac‐cording to the result of method verification ,related substances could be examined by HPLC .Lidocaine hydrochloride was as‐sayed by HPLC ,which showed excellent linearity at the range of 373 .62‐3 736 .19 μg/ml .The average recoveries were 102 .1% (RSD=0 .9% ) .Conclusion The improved standard could be used to control the quality of lidocaine hydrochloride injection .
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Objective: To develop a new method for the simultaneous determination of two hydrophilic components and two lipophilic components of Radix et Rhizoma Salviae Miltiorrhizae. Methods: The HPLC-DAD method was employed using a column of Agilent Zorbax TC C18 (4.6 mm × 250 mm, 5 μm) with a mobile phase of methanol -2% acetic acid. The gradient elution program was as follow:0-15 min, 30% B-40% B; 15-20 min, 40% B-60% B; 20-25 min, 60% B-90% B; 25-40 min, 90% B. The detection wavelength was set at 281 nm and the temperature was 35°C. Results: The linearity was obtained over 3.76-120.20 μg · ml-1 (r=0.999 9) for rosmarinic acid, 34.20-109 4.5 μg · ml-1 (r=0.999 9) for salviamolic acid B, 0.64-20.32 μg · ml-1 (r=0.999 9) for clyptotanshinon, and 1.02-32.72 μg · ml-1 (r=0.999 6) for tanshinone II A. The RSDs of precision and stability of the sample were both less than 1% in 48 hours. The average recovery was between 99.72%-100.63%. Conclusion: The present method is simple and has satisfactory efficacy; it can simultaneously determine multiple hydrophilic and lipophilic bioactive components in Salvia miltiorrhiza from different areas.
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OBJECTIVE To study the analytic method for assaying of glutaral concentration by enzyme-labeled device at one time.METHODS Controlled solution of glutaral and sample solution were taken out and kept until the room temperature.Optical density value was detected at 450 nm.Content of sample was calculated by comparison with the known concentration of glutaral.RESULTS In the range of 0.75-2.50%,concentration of glutaral had linear relationship with the optical density value.Reproductive test:relative average error was within 2%,RSD≤2.51%;interference test:oxidation-resistant-sodium nitrite could make the result negative error.0.1% Sodium nitrite could make the test result decrease by 1.5% relatively.CONCLUSIONS The method is simple,fast and convenient,with accuracy which has met the requirement of hospital infection monitoring and acceptable interfering range made by additives,which is highly practical.
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Objective: To study and determine the Water-soluble substances of Salvia chinensis. Methods: The constituents of the n-Butanol-soluble portion of the water extractive were isolated and purified by means of Sephadex LH20 column chromatographic methods. HPLC was used to determine the contents. Results: Two compounds were isolated and identified as danshensu and rosmarinic acid. The linear range of danshensu was 1.48～7.40 μg. The average recovery was 102.8% and RSD was 1.04% ; The linear range of protocatechualdehyde was 0.05～0.26μg. The average recovery was 101.5% and RSD was 0.72%. Conclusion: The method can provide useful references to quality control of Herba Salvia chinensis. Danshensu was firstly isolated from Herba Salvia chinensis.
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OBJECTIVE:To develop an HPLC method for the determination of Tanshinone ⅡA in Lianchuang pills. METHODS:The chromatographic separation was performed on Agilent Zorbax SB-C18 (250mm?4.6mm,5?m) column with column temperature at 25℃. The mobile phased consisted of methanol-water (75∶25) at a flow rate of 1.0mL?min-1.The detection wavelength was set at 270nm.RESULTS:The linear range of Tanshinone ⅡA was 0.020 2～0.202 0?g(r=0.999 9).The average recovery was 99.79%(RSD=1.01%,n=6). CONCLUSION:The method is simple, rapid and accurate, and it could be used for the quality control of Lianchuang pills.
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Objective To extract and separate crude gingerols and to determine the content of [6]-gingerol in crude gingerols.Methods Crude gingerols were separated from the ginger supercritical-CO2 extracts by silica gel dry column chromatography with solvent system of diethyl ether-n-hexane(7:3).The content of [6]-gingerol in crude gingerols was determined by HPLC.Results [6]-gingerol content in the prepared crude gingerols by silica gel dry column chromatography arrived 52.87 %(m/m).[6]-gingerol had a good linearity in the range of 0.512～ 3.075 ? g,r=0.999 9,and the average recovery was 99.19 %,RSD=1.58 % .Conclusion Silica gel dry column chromatography can be used to quickly,effectively prepare crude gingerols,in which [6]-gingerol content is high,and can supply enough material for further research.The liquid chromatographic analysis of [6]-gingerol is simple,reliable,reproducible and can be used for the quality control of crude gingerols.
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AIM: To establish the quality standard for Chanhua Junsitifen Capsule(Paecilomyces cicadae(Miquel) samson). METHODS: Amino acids,adenine,adenosine,uridnine in Chanhua Junsitifen Capsule were identified by TLC and adenosine was determined by HPLC.Chromatographic conditions were adopted as follows:co-lumn: Inertsil C_18(4.6 mm?250 mm,5 ?m),mobile phase: MeOH-0.05 mol/L KH_2PO_4 solution(15∶85),wavelength: 260 nm,flow rate: 1.0 mL/min. RESULTS: The average recovery was 99.60 % and RSD was 0.62 % and the linear range of adenosine was in the range 0.007 475-2.99 ?g. CONCLUSION: This method is simple,rapid with a good reproducibility.This method can be used for the quality control of Chanhua Junsitifen Capsule.
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OBJECTIVE: To compare the contents of main chemical components in prescription granules and decoction of Fructus aurantii immaturus. METHODS: 3 batches of cut crude drugs of Fructus aurantii immaturus were selected to prepare the granules and decoction. The assaying of water soluble extractive was conducted according to the specification of China Pharmacopeia. The assaying of hesperidin and synephrine was conducted by HPLC. RESULTS: There was no obvious difference between water soluble extractive of granules and that of decoction, while the contents of hesperidin and synephrine were higher in the prescription granules than in the decoction. CONCLUSIONS: The results provide supporting basis for the labeled amount of prescription granule of Fructus aurantii immaturus.
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OBJECTIVE: To determine the content of dracorhodin in Diedaqili Tablets by HPLC. METHODS: The separation was performed on Diamonsil TM C18 column. The mobile phase consisted of acetonitril-0. 05mol? L-1 sodium biphosphate solution ( 45∶ 55) with detection wavelength at 440nm and flow rate at 1. 0mL? min-1. RESULTS: The calibration curve of dracorhodin was linear within the range of 0. 122～ 0. 854? g ( r=0. 999 9) , with average recovery at 101. 4% ( RSD=0. 91% ) . CONCLUSION: This method is simple, reliable and reproducible, and suitable for the quality control of Diedaqili Tablets.
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OBJECTIVE: To establish the method for the determination of diosgenin in Di’ ao Xinxuekang Capsule by HP_LC. METHOD: The condition of HPLC was Shim-pack CLC-Sil columm ( 150mm? 6. 0mm) , mobile phase of 2. 0% isopropand in petroleum ether and UV detector at 206nm. RESULTS : The method proved to be linear in the range at 0. 58～ 11. 6? g of diosgenin with correlation coefficient of 0. 999 8. The linear formula was Y=3. 682? 107X+ 1700, The average recovery and recision were 99. 49% , and RSD=0. 12% ( n=5) . CONCLUSION: The method is simple, accurate, specific and can be used to the quality control of the preparation.
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OBJECTIVE: To determine ginsenoside Rg1 and ginsenoside Re in Jiangshen Capsules by HPLC simultaneously. METHODS: The separation was performed on Kromasil-C18 column, the mobile phase consisted of acetonitrile-0. 05% H3PO4 solution ( 21∶ 79) with flow rate of 1. 0mL? min-1 and detection wavelength of 203nm. RESULTS: The linear ranges of ginsenoside Rg1 and ginsenoside Re were 0. 502～ 4. 016? g( r=0. 999 7) and 1. 090～ 8. 720? g( r=0. 999 8) , respectively, with average recovery at 98. 8% ( RSD=1. 24% ) and 99. 4% ( RSD=1. 68% ) , respectively. CONCLUSION: This method is simple, rapid, accurate and reliable, and suitable for the quality control of Jiangshen Capsules.
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OBJECTIVE:To establish a method for content determination of schisandrin and schisandrin B in compound wurenchun capsule by RP-HPLC.METHODS:Column lichrosphere C18 was used,mobile phase of water and MeOH(gradient elution)was set up,the flow rate was 1.0mL?min-1,the column temperature was 30℃and the detection wavelength was 254nm.RESULTS:The linear ranges of schizandrin and schisandrin B were within 0.182 4～1.641 6?g(r=1.000 3)and 0.189 6～ 1.706 4?g(r=0 .999 9),respectively.The average recoveries were 98.32%(RSD=1.02%)and 97.22 %(RSD=0.94%),respectively.CONCLUSION:The established method is convenient,accurate and highly specific,and it can be used for the quality control of compound wurenchun capsule.
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OBJECTIVE:To establish a RP-HPLC method for the determination of baicalin and jasminoidin in Qingkailing Injection.METHODS:It was performed on DiamonsilTM C18 column with acetonitrile-20 mmol?L-1 sodium dihydrogen phosphate solution (20:80)as mobile phase.The flow rate was 1.0 mL?min-1.The detection wavelength was 238 nm.RESULTS:The liner range of baicalin was 1～50?g?mL-1,(r=0.999 5)and the average recovery was 100.75%(RSD=1.75%);The liner range of jasminoidin was 0.1～10?g?mL-1(r=0.999 7)and the average recovery was 100.63%(RSD=1.35%).CONCLUSION:This method is rapid,simple,accurate and sensitive.It can be used for quality control of Qingkailing Injection.
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OBJECTIVE:To determine Sarsasapogenin in Jujube seed concentrated pills by RP-HPLC-ELSD.METHODS:Separation of Sarsasapogenin was performed on Zorbax C18 column with methanol-water (90:10)as a mobile phase at a flow rate of 1.0mL?min-1.The temperature of the drift tube was 85℃and the air flow-rate was at 1.71mL?min-1.RESULTS:The linear range of Sarsasapogenin was 0.112 7～0.676 2mg?mL-1(r=0.998 3).The average recovery was 99.83%(RSD=0.93%).CONCLUSION:The method is simple,accurate and reproducible,and suitable for the quality control of Jujube seed concentrated pills.
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OBJECTIVE:To set up a HPLC method for the determination of the contents of notoginsenoside R1,ginsenoside Rg1 and Rb1 in Sanqishangyao tablets.METHODS:It was performed on VP-ODS (150mm?4.6mm,5?m),and the mobile phase was acetonitrile-water with gradient elution system(0～20min(20∶80),20～26min(40∶60),26～35min(20∶80)).The flow rate was 1.0mL?min-1 and the column temperature was room temperature.The detection wavelength was 203nm.RESULTS:The liner range of notoginsenoside R1 was 0.261～7.83?g(r=0.999 9)and the average recovery was (101.12?2.03)%(RSD=2.1%).The liner range of ginsenoside Rg1 was 0.602 5～18.075?g(r=0.999 7)and the average recovery rate was (97.22?3.33)%(RSD=1.9%).The liner range of ginsenoside Rb1 was 0.537 5～16.125?g(r=0.999 6)and the average recovery rate was(100.71?2.4)%(RSD=1.6%).CONCLUSION:The method is suitable for the content determination of notoginsenoside R1,ginsenoside Rg1 and Rb1 in Sanqishangyao Tablets.
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OBJECTIVE:To establish HPLC method for the simultaneous assaying of paracetamol and caffeine in ankahua_ngmin capsules.METHODS:The determination was performed on phenomenex luna C18 column under room temperature;the mobile phase consisted of methanol-water(24∶76) with a flow rate at 1.0ml/min,detecting wavelength at 215 nm and sensibility at 0.01AUFS.RESULTS:The linear ranges for paracetamol and caffeine were 50～250?g/ml(r=0.9 999) and 5.0～25?g/ml(r=0.9 999),respectively.The average recoveries were 100.7%(RSD=1.8%)and 101.4%(RSD=1.4%),respectively.CONCLUSION:This method is simple,rapid and accurate,which can substitute for titration in the assaying of ankahua_ngmin capsules.
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OBJECTIVE:To compare the effects of2different treatment methods on the assaying of triptolide alcohol in tripterygium wilfordii cut crude drug.METHODS:After concentration,tripterygium wilfordii cut crude drug water decoction underwent column chromatographic separation after adsorption with neutral alumina(Method1)and neutral alumina column chromatographic separation after ethanol precipitation and extraction by chloroform(Method2),respectively.Triptolide alcohol was determined by HPLC and the assaying result underwent pairing and t tests.RESULTS:There was significant difference between the2methods with the content determined by Method1significantly higher than that by Method2(P