الملخص
Abstract To assess the effect of different whitening toothpastes on enamel surface morphology, chemical profile and their whitening efficiency. Sixty teeth were divided into 5 groups (12 teeth/group); Gp I: brushed with no toothpaste. Gp II: brushed with Pearl-based toothpaste. Gp III: brushed with Charcoal- based toothpaste. Gp IV: brushed with Alumina-based toothpaste. Gp V: brushed with salt and lemon- based toothpaste. Each tooth was brushed with a bean sized toothpaste wetted with distilled water twice daily by using standard electronic toothbrush for four weeks. Enamel surface morphology, chemical profile and color of each tooth were investigated. Chemical profile results and color measurements were analyzed statistically. Gp I revealed normal enamel surface morphology and chemical profile. Gp II and Gp III demonstrated surface morphology close to Gp I with insignificant reduction in mineral content. Gp IV showed obvious shallowing of perikymata ridges, exposure of fish-scale appearance, with pits and depressions, alongside to the significant reduction in mineral content. Gp V presented the most enamel surface alteration with widening of prism sheath and depressions all over the surface, besides the highest significant reduction in mineral content. Gp V, followed by Gp IV, demonstrated the highest color and whiteness changes, followed by Gp III, then Gp II, while the lowest value was in Gp I. Salt & lemon-based toothpaste, followed by Alumina-based, exerted the most considerable changes in the morphology and chemical profile of the enamel surface, beside to the higher whitening effects on teeth than the others.
Resumen El objetivo del presente estudio fue evaluar el efecto de diferentes pastas dentales blanqueadoras sobre la morfología y el perfil químico de la superficie del esmalte y su eficacia blanqueadora. Sesenta dientes se dividieron en 5 grupos (12 dientes/grupo); Grupo I: cepillado sin pasta de dientes. Grupo II: cepillado con pasta de dientes a base de perlas. Grupo III: cepillado con pasta de dientes a base de carbón. Grupo IV: cepillado con pasta de dientes a base de Alúmina. Grupo V: cepillado con sal y pasta de dientes a base de limón. Cada diente se cepilló con una pasta de dientes del tamaño de un frijol humedecida con agua destilada dos veces al día utilizando un cepillo de dientes electrónico estándar durante cuatro semanas. Se investigaron la morfología de la superficie del esmalte, el perfil químico y el color de cada diente. Los resultados del perfil químico y las mediciones de color se analizaron estadísticamente. El Grupo I reveló una morfología de la superficie del esmalte y un perfil químico normales. Los Grupos II y III demostraron una morfología de superficie cercana a la del Grupo I con una reducción insignificante en el contenido mineral. El grupo IV mostró una evidente reducción de las crestas perikymatas, exposición de apariencia de escamas de pez, con hoyos y depresiones, junto con una reducción significativa en el contenido mineral. El grupo V presentó la mayor alteración de la superficie del esmalte con ensanchamiento de la vaina del prisma y depresiones en toda la superficie, además de una significativa reducción en el contenido mineral. El grupo V, seguido del grupo IV, demostró los mayores cambios de color y blancura, seguido del grupo III, luego el grupo II, mientras que el valor más bajo se presentó en el grupo I. Las pastas dentales a base de sal y limón, seguidas de las de alúmina, ejercieron los cambios más considerables en la morfología y el perfil químico de la superficie del esmalte, además de tener mayores efectos blanqueadores sobre los dientes que las demás.
الموضوعات
Tooth Bleaching/methods , Toothpastes/analysis , Dental Enamel , In Vitro Techniques , Costa Ricaالملخص
Abstract Introduction: The sea urchin Diadema mexicanum, due to its bioerosion activity, is considered of ecological importance. This phenomenon could negatively or positively affect coral reef ecosystems. The bioerosion process varies according to the abundance and size of the sea urchin. Objective: Juvenile organisms possess different metabolic needs compared to adults, so knowing their stomach content according to size allows us to quantify the selection of substrate bioeroded. Methods: To determine this, D. mexicanum individuals were collected in 12 sites from January 2009 to September 2010 along the Eastern Tropical Pacific coast. The stomach content was categorized in Carbonated Fraction (CF), Non-Carbonated Fraction (NCF), and Organic Matter (OM). Stomach content was analyzed according to a) juvenile (< 2.5 cm) or adult (> 2.5 cm) stage and b) locality. Results: Juveniles presented the following stomach content average percentages: 20.7 % OM, 12 % NCF and 67.9 % CF; and adults: 11.4 % OM, 14.8 % NCF and 73.8 % CF. Based on a Wilcoxon test and a Kendall linear regression, the following results were obtained. The carbonated fraction in the stomach increased by 0.47 units on average for every cm of growth (p < 0.05). OM consumed by D. mexicanum increases only 0.05 units for every cm of growth (p < 0.05). We found a difference of stomach content depending on the site (p < 0.05) and life stage (p < 0.05). Localities like Huatulco and Coco presented significant differences that could be related to local oceanographic conditions. Conclusions: We relate these changes of the stomach fractions to the necessity of the juvenile sea urchins for nutrients to maintain their growth. The amount of OM is crucial for the development of early stages, meaning that there is a difference in substrate selection associated with growth.
Resumen Introducción: El erizo de mar Diadema mexicanum, por su actividad de bioerosión, es considerado de importancia ecológica. Este fenómeno podría afectar negativa o positivamente a los ecosistemas de arrecifes de coral. El proceso de bioerosión varía según la abundancia y el tamaño del erizo de mar. Objetivo: Los organismos juveniles poseen diferentes necesidades metabólicas en comparación con los adultos, por lo que conocer el contenido estomacal según el tamaño, nos permite cuantificar la selección de sustrato bioerosionado. Métodos: Para determinar esto, se recolectaron individuos de D. mexicanum en 12 sitios desde enero de 2009 hasta septiembre de 2010 a lo largo de la costa del Pacífico Tropical Oriental. El contenido estomacal se clasificó en Fracción Carbonatada (FC), Fracción No Carbonatada (NCF) y Materia Orgánica (MO). El contenido estomacal se analizó según a) estadio juvenil (< 3 cm) o adulto (> 3 cm) y b) localidad. Resultados: Los juveniles presentaron los siguientes porcentajes promedio del contenido estomacal: 20.7 % OM, 12 % NCF y 67.9 % CF; y adultos: 11.4 % OM, 14.8 % NCF y 73.8 % CF. Con base en una prueba de Wilcoxon y una regresión lineal de Kendall, se obtuvieron los siguientes resultados. La fracción carbonatada en el estómago aumentó en promedio 0.47 unidades por cada cm de crecimiento (p < 0.05). La MO consumida por D. mexicanum aumenta solo 0.05 unidades por cada cm de crecimiento (p < 0.05). Encontramos una diferencia en el contenido estomacal según el sitio (p < 0.05) y el estadio de vida (P < 0.05). Localidades como Huatulco y Coco presentaron diferencias significativas que podrían estar relacionadas con las condiciones oceanográficas locales. Conclusiones: Relacionamos estos cambios de la composición porcentual del contenido estomacal con la necesidad de los erizos de mar juveniles de nutrientes para mantener su crecimiento. La cantidad de MO es crucial para el desarrollo de las primeras etapas, lo que significa que existe una diferencia en la selección de sustrato asociada con el crecimiento.
الموضوعات
Animals , Sea Urchins/growth & development , Beach Erosion , Coral Reefs , Dietالملخص
Objective To establish method for simultaneous determination of hesperidin, cinnamaldehyde and eugenol in Chunyang Zhengqi capsules by high performance liquid chromatography. Methods The column was Agilent PorosheⅡ 120 EC-C18 (4.6 mm×150 mm, 4 μm). The mobile phase was acetonitrile-water with gradient elution. The column temperature was 35℃. The flow rate was 1.0 ml/min, and the detection wavelength was 284 nm. Results The methodological verification showed that hesperidin, cinnamaldehyde and eugenol had a good linearity (r≥0.999 9). The precisions were less than 2.0%. The average recovery was between 98.0% and 101.9%. The stability and repeatability of RSD were also less than 3.0%, which met the requirements of method validation. Conclusion The method is simple, stable, reproducible and accurate, which could be used to the quality control of Chunyang Zhengqi capsules.
الملخص
Objective To establish the method for content determination of three lignans of Dendrobium Fimbriatum Hook..Methods The lignans in Dendrobium tasselii were identified by high-performance liquid chromatography/multi-stage mass spectrometry(HPLC-ESI/MSn)coupled with ultraviolet absorption spectrometry(UV)coupled with retention time localization of high-performance liquid chromatography(HPLC).The separation was carried out on a Kromasil 100-5 C18 column(4.6 mm×250 mm,5 μm)using a gradient elution of acetonitrile-0.1%formic acid solution as the mobile phase,the volume flow rate was 0.8 mL·min-1 and the column temperature was 35℃,and the mass spectrometry was performed using an ESI ion source with the data collected in the negative ion mode.The HPLC content was determined on the same column as that of MS analysis,with the mobile phase methanol + acetonitrile(V/V=1∶1)-0.01 mol/L ammonium acetate solution,gradient elution,flow rate of 0.8 mL·min-1,column temperature of 40℃,and detection wavelength of 215 nm.Results Syringaresinol di-O-glucoside and(-)-Syringaresinol 4-O-β-D-glucopyranoside and DL-Syringaresinol were identified from Dendrobium fimbriatum Hook.,and the results of content determination showed that the linear ranges of above three components were respectively 0.1701-3.4020,0.1020-2.0400,0.0403-0.8060 μg(r≥0.9995),the average recoveries were in the range of 97.71%-101.67%,and the relative standard deviations(RSDs)were all less than 3.0%.The contents of Syringaresinol di-O-glucoside and(-)-Syringaresinol 4-O-β-D-glucopyranoside and DL-Syringaresinol in the 10 batches of samples were 0.7779-1.3852,0.0734-0.1966,0.0295-0.1882 mg·g-1.Conclusion This research method can provide a reference basis for the quality evaluation method of Dendrobium fimbriatum Hook..
الملخص
ObjectiveTaking Achyranthis Bidentatae Radix（ABR） from different origins as samples， to quantitatively analyze the chemical composition and chromaticity of ABR with different processing degrees， and clarify the correlation and change law between color and composition in the processing process of ABR， so as to provide reference for the quality evaluation of processed products of ABR. MethodThe colorimeter is used to measure the chromaticity values of three kinds of processing degrees of ABR in different origins to show the color value change trend during the processing process， and the color parameters of wine-processed and salt-processed products of ABR with different processing degrees were analyzed by principal component analysis（PCA）， orthogonal partial least squares-discriminant analysis（OPLS-DA） and other analysis methods. The contents of eight representative components of ABR were measured by high performance liquid chromatography（HPLC）， the correlation between chromaticity and each representative component was analyzed by Pearson correlation analysis， and the applicability of the selected eight representative components was further verified by Fisher linear discriminant analysis， and the wine-processed and salt-processed products of ABR with different processing degrees were grouped according to the degree of processing， and 48 samples of wine-processed and salt-processed products with different processing degrees were used as training samples. Taking the contents of 5-hydroxymethylfurfural， polypodine B， β-ecdysterone， 25R-inokosterone， 25S-inokosterone， ginsenoside Ro， chikusetsusaponin Ⅳa and polysaccharides as variables， the discriminant function was established respectively， and 12 samples of wine-processed and salt-processed products of ABR with different processing degrees were back-tested to verify the discriminant function and test the reliability of the function. ResultPCA and OPLS-DA results showed that ABR samples with different processing degrees were classified into clusters， and the results could significantly distinguish different processed products. During the process of wine and salt processing， the contents of 5-hydroxymethylfurfural， ginsenoside Ro， and chikusetsusaponin Ⅳa gradually increased with the deepening of the processing degree， while the contents of polypodine B， β-ecdysterone， 25R-inokosterone， 25S-inokosterone and polysaccharides showed a gradual decreasing trend， indicating these 8 components increased and decreased to different degrees in the process of wine and salt processing. The results of Pearson correlation analysis showed that the 5-hydroxymethylfurfural content of the samples with different processing degrees of wine-processed and salt-processed products were negatively correlated with the brightness value（L*） and the total color difference value（E*ab）（P<0.01）， and positively correlated with the red-green value（a*） and the yellow-blue value（b*）（P<0.01）， and that the content of polypodine B and polysaccharides were positively correlated with L* and E*ab（P<0.01）. The discriminant functions of wine-processed and salt-processed products of ABR were established by Fisher linear discriminant analysis， and their accuracy rates in the training samples were 93.75% and 95.83%， respectively. Twelve test samples of wine-processed and salt-processed products with different processing degree were back substitution， and the correct rate was 100%. ConclusionThe trend of composition and color changes of ABR with different processing degrees in different production areas is relatively consistent， and the color value can better distinguish ABR with different processing degrees， and the color of ABR is related to some representative components in the processing process， indicating that the color can provide reference for the identification of the processing degree of ABR and the prediction of component content.
الملخص
ObjectiveTo improve the quality standard of Yuanhu Zhitong oral liquid in order to strengthen the quality control of this oral liquid. MethodThin layer chromatography（TLC） was used for the qualitative identification of Corydalis Rhizoma and Angelicae Dahuricae Radix in Yuanhu Zhitong oral liquid by taking tetrahydropalmatine， corydaline reference substances and Corydalis Rhizoma reference medicinal materials as reference， and cyclohexane-trichloromethane-methanol（5∶3∶0.5） as developing solvent， Corydalis Rhizoma was identified using GF254 glass thin layer plate under ultraviolet light（365 nm）. And taking petroleum ether（60-90 ℃） -ether-formic acid（10∶10∶1） as developing solvent， Angelicae Dahuricae Radix was identified using a silica gel G TLC plate under ultraviolet light（305 nm）. High performance liquid chromatography（HPLC） was performed on a Waters XSelect HSS T3 column（4.6 mm×250 mm， 5 μm） with acetonitrile（A）-0.1% glacial acetic acid solution（adjusted pH to 6.1 by triethylamine）（B） as the mobile phase for gradient elution（0-10 min， 20%-30%A； 10-25 min， 30%-40%A； 25-40 min， 40%-50%A； 40-60 min， 50%-60%A）， the detection wavelength was set at 280 nm， then the fingerprint of Yuanhu Zhitong oral liquid was established， and the contents of tetrahydropalmatine and corydaline were determined. ResultIn the thin layer chromatograms， the corresponding spots of Yuanhu Zhitong oral liquid， the reference substances and reference medicinal materials were clear， with good separation and strong specificity. A total of 12 common peaks were identified in 10 batches of Yuanhu Zhitong oral liquid samples， and the peaks of berberine hydrochloride， dehydrocorydaline， glaucine， tetrahydropalmatine and corydaline. The similarities between the 10 batches of samples and the control fingerprint were all >0.90. The results of determination showed that the concentrations of corydaline and tetrahydropalmatine had good linearity with paek area in the range of 0.038 6-0.193 0， 0.034 0-0.170 0 g·L-1， respectively. The methodological investigation was qualified， and the contents of corydaline and tetrahydropalmatine in 10 batches of Yuanhu Zhitong oral liquid samples were 0.077 5-0.142 9、0.126 1-0.178 2 g·L-1， respectively. ConclusionThe established TLC， fingerprint and determination are simple， specific and reproducible， which can be used to improve the quality control standard of Yuanhu Zhitong oral liquid.
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OBJECTIVE To establish an HPLC fingerprint of Xiao’er resuqing oral liquid， and to determine the contents of twelve index components. METHODS HPLC method was adopted. The determination was performed on Venusil MP C18 column with mobile phase consisting of acetonitrile-0.1% phosphate aqueous solution （gradient elution） at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm， the column temperature was 30 ℃， the injection volume was 10 μL. HPLC fingerprint of Xiao’er resuqing oral liquid was established by using the Similarity Evaluation System of Chromatographic Fingerprint of TCM （2012 edition） to evaluate the similarity. The contents of 12 components were determined， including （R， S）-goitrin， 3，5-O-dicaffeoyl quinic acid， puerarin， forsythin， forsythoside A， chlorogenic acid， baicalin， saikosaponins d， wogonoside， baicalein， emodin and chrysophanol. RESULTS The similarity of HPLC fingerprints of 13 batches of Xiao’er resuqing oral liquid was greater than 0.97， and 14 common peaks were confirmed. The contents of the above 12 index components in 13 batches of Xiao’er resuqing oral liquid were as follows： 0.078-0.172， 1.564-2.736， 1.338-2.578， 0.426-0.872， 1.477-2.628， 1.396-2.447， 4.052-9.146， 0.367- 0.692， 1.974-4.674， 1.274-2.969， 0.085-0.167 and 0.155-0.307 mg/mL. CONCLUSIONS The established HPLC fingerprint and content determination methods have high accuracy and high specificity， which can be used for the quality evaluation of Xiao’er resuqing oral liquid.
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OBJECTIVE To establish a method for the content determination of 11 components such as protodioscin in Guge fengtong tablets， and to evaluate the comprehensive quality of Guge fengtong tablets by combining with chemometric analysis and entropy weight-technique for order preference by similarity to ideal solution （EW-TOPSIS） method. METHODS HPLC method was adopted. The determination was performed on Agilent Eclipse Plus C18 column with a mobile phase consisted of acetonitrile- 0.2% phosphoric acid solution at the flow rate of 1.0 mL/min by gradient elution. The column temperature was set at 30 ℃ . The detection wavelengths were set at 203 nm （0-28 min， protodioscin， methyl protodioscin， pseudoprotodioscin， dioscin） and 280 nm （28-60 min， catechin， epicatechin， liquiritigenin， medicarpin， 6-gingerol， 8-gingerol， 10-gingerol）； the sample size was 10 μL. Using epicatechin as the internal reference， quantitative analysis of multi-components by single marker （QAMS） method was used to determine the contents of protodioscin， methyl protodioscin， pseudoprotodioscin， dioscin， catechin， liquiritigenin， medicarpin， 6-gingerol， 8-gingerol and 10-gingerol， which were compared with the results of the external standard method. SPSS 26.0 software and SIMCA 14.1 software were used for principal component analysis and orthogonal partial least squares-discriminant analysis， with variable importance in projection （VIP） value greater than 1 as the standard， to screen for differential markers that affect the quality； the EW-TOPSIS method was adopted to evaluate the quality of 15 batches of samples comprehensively.RESULTS The contents of protodioscin， methyl protodioscin， pseudoprotodioscin， dioscin， catechin， liquiritigenin， medi-carpin， 6-gingerol， 8-gingerol and 10-gingerol determined by HPLC combined with QAMS were 6.330-10.863， 1.150-2.274， 0.431- 0.740， 2.818-4.823， 0.826-1.510， 0.043-0.094， 0.079-0.231， 0.479-1.020， 0.146-0.288， 0.118-0.318 mg/g， respectively； there were no statistical significances， compared with the external standard method （P＞0.05）. A total of 15 batches of samples were clustered into 3 groups， with S1-S6， S7-S10， and S11-S15 clustered into one group， respectively. The VIP values of protodioscin， epicatechin， dioscin and 6-gingerol were greater than 1. Euclidean closeness values of the optimal solution （C）i for 15 batches of samples were 0.163 5 to 0.703 7， and Ci values of S11-S15 were all higher than 0.6. CONCLUSIONS The established QAMS method is accurate and simple， and can be used for comprehensive quality evaluation of Guge fengtong tablets， by combining with chemometric analysis and EW-TOPSIS method. Protodioscin， epicatechin， dioscin and 6-gingerol are the differential markers that affect the quality of Guge fengtong tablets. Samples S11-S15 have better quality.
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Objective:To evaluate the effect of individualized positive end-expiratory pressure (PEEP) titration based on open-lung strategy on the intraoperative thoracic fluid content (TFC) in elderly patients undergoing transurethral ultrasound-guided laser-induced prostatectomy (TULIP).Methods:Eighty-six American Society of Anesthesiologists Physical Status classification Ⅱ or Ⅲ, patients, aged 65-80 yr, with body mass index of 18-28 kg/m 2, scheduled for elective TULIP, were divided into 2 groups ( n=43 each) by the random number table method: fixed PEEP group (group C) and individualized PEEP titration group (group P). PEEP was set at 4 cmH 2O after routine mechanical ventilation in group C. Patients underwent pulmonary recruitment maneuvers combined with individualized PEEP titration during surgery in group P. TFC was measured using a non-invasive cardiac output monitor at 5 min after tracheal intubation (T 0), 30 min after PEEP titration and ventilation (T 1), 5 min before surgery (T 2), and 5 min before leaving the recovery room (T 3). Cardiac output, oxygenation index and stroke volume index were recorded from T 0-T 2, arterial blood gas analysis was simultaneously performed to record peak airway pressure and dynamic lung compliance, and oxygenation index was calculated. The duration of postanesthesia care unit stay, pulmonary complications within 7 days after surgery, and length of hospital stay were also recorded. Results:Eighty-three patients were finally included, with 42 in group C and 41 in group P. Compared with group C, TFC was significantly decreased at T 1-T 3, cardiac index, cardiac output and stroke volume index were decreased at T 1, dynamic lung compliance, PaO 2 and oxygenation index were increased at T 1 and T 2, PaCO 2 was decreased, the incidence of postoperative pulmonary complications was reduced, and the duration of postanesthesia care unit stay and postoperative length of hospital stay were shortened in group P ( P<0.05). Conclusions:Individualized PEEP titration based on open-lung strategy can effectively decrease TFC and improve intraoperative oxygenation and prognosis in elderly patients undergoing TULIP.
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AIM To establish an HPLC method for the simultaneous content determination of gallic acid,protocatechuic acid,morroniside,loganin,sweroside,paeoniflorin,hypericin,astragalin,salvianolic acid B,salvianolic acid A,epimedin C and icariin in Bushen Huoxue Sanjie Capsules.METHODS The analysis was performed on a 30℃thermostatic Agilent 5 TC-C18 column(250 mm×4.6 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1%phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 240 nm.RESULTS Twelve constituents showed good linear relationships within their own ranges(r≥0.999 8),whose average recoveries were 97.11%-101.14%with the RSDs of 0.60%-2.65%.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of Bushen Huoxue Sanjie Capsules.
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AIM To establish an HPLC method for the simultaneous content determination of urine,guanosine,adenosine,(R,S)-hysterone,chlorogenic acid,forsythian glycoside A,luteolin,3,5-dicaffeioyl quinic acid,4,5-dicaffeioyl quinic acid and phillyrin in Xiao'er Ganmao Granules.METHODS The analysis was performed on a 40℃thermostatic Welchrom C18 column(4.6 mm×250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.2%glacial acetic acid flowing at 0.8,1.0 mL/min in a gradient elution manner,and the detection wavelengths were set at 230,254,327 nm.RESULTS Ten constituents showed good linear relationships within their own ranges(r≥0.999 0),whose average recoveries were 93.68%-98.08%with the RSDs of 0.90%-1.86%.CONCLUSION This stable and reliable method can be used for the quality control of Xiao'er Ganmao Granules.
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AIM To establish a UPLC method for the simultaneous content determination of schisandrol A,gomisin J,schisandrol B,angeloylgomisin H,angeloylgomisin Q,schisanhenol,deoxyschizandrin and schisandrin C in Waigan Fenghan Granules.METHODS The analysis was performed on a 40℃thermostatic WELCH Ultimate?-C18 column(100 mm×2.1 mm,1.8 μm),with the mobile phase comprising of acetonitrile-0.1%formic acid flowing at 0.3 mL/min in a gradient elution manner,and the detection wavelength was set at 267 nm.RESULTS Eight Schisandra lignans showed good linear relationships within their own ranges(R2≥0.998 3),whose average recoveries were 96.47%-104.96%with the RSDs of 0.62%-1.60%.CONCLUSION This simple,rapid and accurate method can be used for the quality control of Hugan Tablets.
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AIM To analyze the component composition of Xeriga-4 Powder,and to determine the contents of phellodendrine,chlorogenic acid,gardenoside,berberine,rutin and curcumin.METHODS The high performance liquid chromatography-Q-exactive orbitrap mass spectrometry(HPLC-Q-Exactive-MS)qualitative analysis was performed on a 35℃thermostatic Agilent ZORBAX SB-Aq column(4.6 mm×150 mm,5 μm),with the mobile phase comprising of methanol-0.1%formic acid flowing at 0.35 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning.High performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)quantitative analysis was performed on a 35℃thermostatic Shim-pack GIST-HP C18 column(2.1 mm×100 mm,3 μm),with the mobile phase comprising of methanol-0.1%formic acid flowing at 0.25 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning with multiple reaction monitoring mode.RESULTS Total 65 constituents were identified,containing 19 alkaloids,13 organic acids,13 flavonoids,7 curcumins,6 iridoids,4 fatty acids,2 aldehydes,and 1 amino acid.Six constituents showed good linear relationships within their own ranges(r≥0.999 1),whose average recoveries were 96.44%-102.37%with the RSDs of 2.05%-3.74%.CONCLUSION This study can provide a reference for the quality control for Xieriga-4 Powder.
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AIM To establish an UPLC-MS/MS method for simultaneous content determination of protocatechuic acid,epicatechin,chlorogenic acid,quercitrin,gaultherin and gaultheroside A in Gaultheria leucocarpa var.yunnanensis.METHODS The analysis was performed on a 40℃thermostatic Waters BEH C18 column(100 mm×2.1 mm,1.7 μm),with the mobile phase comprising of water(containing 0.1%formic acid)-acetonitrile(containing 0.1%formic acid)flowing at 0.3 mL/min in a gradient elution manner,and electron spray inoization source was adopted in positive and negative ion scanning with multiple reaction monitoring(MRM)mode.Hierarchical cluster analysis(HCA)and principal component analysis(PCA)was used to screen important components that affect the quality of medicinal materials.RESULTS Six constituents showed good linear relationships within their own ranges(R2≥0.998 2),whose average recoveries were 98.76%-101.88%with the RSDs of 1.0%-2.5%.The constituents of G.leucocarpa in the roots and aerial parts were quite different.Gaultherin,epicatechin and protocatechuic acid may be the quality mark constituents of G.leucocarpa.CONCLUSION This accurate and efficient method can be used for the quality control of G.leucocarpa.
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AIM To investigate the effects of different compatibility ratios and processing method on the content of rutin,isoquercetin,ferulic acid,quercetin,isotoosendanin,kaempferol,toosendanin,α-pinene,trans-anethole in the combination use of Toosendan Fructus and Foeniculi Fructus,and to explore the optimal compatibility ratio for its use.METHODS The analysis of HPLC-DAD was performed on a 30℃thermostatic ZORBAX SB C18 column(4.6 mm×250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1%phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the use of DAD detector.SPSS 24.0 software was used to analyze the data differences.RESULTS Nine constituents showed good linear relationships within their own ranges(r≥0.999 1),whose average recoveries were 96.19%-103.13%with the RSDs of 1.86%-2.67%.Generally higher total content of nine constituents were detected in the combination use groups when Toosendan Fructus-Foeniculi Fructus were at ratios of 1 ∶ 1,1 ∶ 2,and 2 ∶ 1 than those single uses(P<0.05),and among which the 1 ∶ 1 ratio contributed the highest total content.After salt processing,decreased content of toosendanin and isotoosendanin,α-pinene and trans-anethole(P<0.05,P<0.01)),increased isoquercetin content(P<0.01),and no significant content changes of other ingredients were detected.CONCLUSION Through this method of high accuracy and good reproducibility,we learn that the combination use of Toosendan Fructus and Foeniculi Fructus promotes the dissolution of the nine constituents,and the maximum content is achieved at ratio of 1 ∶ 1.
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AIM To establish a UPLC-MS/MS method for the simultaneous content determination of liquiritin apioside,alibiflorin,swertiamarin,methyl gallate,benzoylpaeoniflorin,sweroside,6′-O-β-D-glucosylgentiopicroside,isoliquiritigenin,loganic acid,liquiritigenin,gallic acid,paeoniflorin,oxypaeoniflorin,gentiopicroside,glycyrrhizic acid,isoliquiritoside and liquiritin in Yangxue Ruanjian Capsules.METHODS The analysis was performed on a 40℃thermostatic Waters BEH C18column(2.1 mm×100 mm,1.7 μm),with the mobile phase comprising of 2 mmol/L ammonium acetate(containing 0.1%formic acid)-acetonitrile flowing at 0.3 mL/min in a gradient elution manner,and electron spray ionization source was adopted in negative ion scanning with multiple reaction monitoring mode.RESULTS Seventeen constituents showed good linear relationships within their own ranges(r>0.999 6),whose average recoveries were 91.33%-104.03%with the RSDs of 1.58%-3.50%.CONCLUSION This rapid,accurate and stable method can be used for the quality control of Yangxue Ruanjian Capsules.
الملخص
AIM To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous content determination of gastrodin,parishin E,syringin,parishin B,parishin C,ferulic acid,parishin A,buddleoside,harpagoside and cinnamic acid in Tianma Toufengling Capsules.METHODS The analysis was performed on a 30℃thermostatic GL Science InertsilTM ODS-3 column(150 mm×4.6 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1%phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelengths were set at 220,280 nm.Syringin was used as an internal standard to calculate the relative correction factors of the other nine constituents,after which the content determination was made.RESULTS Ten constituents showed good linear relationships within their own ranges(r≥0.999 7),whose average recoveries were 98.53%-102.22%with the RSDs of 1.26%-2.68%.The result obtained by QAMS approximated those obtained by external standard method.CONCLUSION This accurate and specific method can be used for the quality control of Tianma Toufengling Capsules.
الملخص
AIM To simultaneously determine the contents of neochlorogenic acid,caffeic acid,chlorogenic acid,cryptochlorogenic acid,hydroxysafflor yellow A,ferulic acid,senkyunolide I,senkyunolide H and senkyunolide A in Fuyang Granules,and to make chemical pattern recognition.METHODS The UHPLC was performed on a 35℃thermostatic Waters Acquity UPLC?BEH C18 column(150 mm×2.1 mm,1.7 μm),with the mobile phase comprising of acetonitrile-0.01%phosphoric acid flowing at 0.4 mL/min in a gradient elution manner,and the detection wavelengths were set at 278,322,325,390 nm.Then heatmap clustering analysis and principal component analysis were adopted.RESULTS Nine constituents showed good linear relationships within their own ranges(r>0.999 0),whose average recoveries were 93.89%-102.25%with the RSDs of 0.85%-2.88%.Different batches of samples from the same enterprises demonstrated consistent overall qualities,while the overall qualities of samples from different enterprises exhibited obvious differences.CONCLUSION This simple and accurate method can be used for the quality control of Fuyang Granules.
الملخص
AIM To investigate the influencing factors in scale-up of extraction process for Yunpi Xiaoshi Prescription.METHODS HPLC was adopted in the content determination of catechin,ferulic acid,taxifolin,isovitexin,narirutin,atractylenolideⅡ,naringin,morin,hesperidin,luteolin,hederagenin,atractylenolideⅠ,naringenin and hesperetin,the fingerprints were established,after which the effects of container volume,optimal fire and feeding quantity on the contents of various constituents were evaluated.RESULTS Fifteen batches of samples demonstrated the similarities of more than 0.995.Fourteen constituents showed good linear relationships within their own ranges(r>0.999 0),whose average recoveries were 96.4%-103.3%with the RSDs of 0.5%-2.7%.The influencing degree of optimal fire was greater than that of container volume and feeding quantity.CONCLUSION The combination of multi-component content determination and fingerprints can provide data basis and theoretical reference for the technology of consistency evaluation in scale-up of extraction process for Yunpi Xiaoshi Prescription.
الملخص
AIM To determine the contents of aspartic acid,glutamic acid,serine,glycine,threonine,citrulline,arginine,alanine,γ-amino-butyric acid,tyrosine,valine,phenlalanine,isoleucine,ornithine,leucine,lysine and proline in Gualoupi Injection and its intermediates,and to analyze their change laws.METHODS The OPA-FMOC online derivatization analysis was performed on a 45℃ thermostatic Waters XBridge C18 column(4.6 mm×100 mm,3.5 μm),with the mobile phase comprising of phosphate buffer solution-[methanol-acetonitrile-water(45 : 45 : 10)]flowing at 1 mL/min in a gradient elution manner,and the detection wavelengths were set at 262,338 nm.Principal component analysis and heatmap analysis were adopted in chemical pattern recognition for the corresponding intermediates in ten processes of six batches of samples.RESULTS Seventeen amino acids showed good linear relationships within their own ranges(R2>0.998 0),whose average recoveries were 83.4％-119.5％with the RSDs of 0.91％-7.94％.Different batches of samples in the same process were clustered,and the corresponding intermediates in different processed were clustered into three groups.Alcohol precipitation and cation exchange column demonstrated the biggest influences on amino acid composition.CONCLUSION This experiment can provide important references for the critical factors on quality control of Gualoupi Injection,thus ensure the stability and uniformity of final product.