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Objective:To establish the TLC identification method and content determination method of ferulic acid, ligustilide, hydroxysafflor yellow A and paeoniflorin in Shangke Huoxue Decoction for quality evaluation.Methods:Ferulic acid, ligustilide, hydroxysafflor yellow A and paeoniflorin were qualitatively identified by TLC method, and the content was determined by HPLC method. Waters Symmetry ShieldTM RP18 column (4.6 mm×250 mm, 5 μm) was set, the mobile phase consisted of acetonitrile-0.15% phosphoric acid water with gradient elution at a flow of 1.0 ml/min, and the column temperature was 30 ℃.The detection wavelength was 320 nm (33-50 min for ferulic acid, 55-70 min for ligustilide), 403 nm (7-31 min for hydroxysafflor yellow A) and 230 nm (7-31 min for paeoniflorin).Results:The TLC spots were clear. The linear relationships of ferulic acid, ligustilide, and hydroxysafflor yellow A were good in the range of 3.05-48.74 μg, 3.50-26.24 μg, 21.34-213.44 μg. The method was stable, repeatable with good recovery rate.Conclusion:The TLC and HPLC method for the simutanous determination of the four effective components in Shangke Huoxue Decoction were established, and the methods are suitable for the quality evaluation of Shangke Huoxue Decoction.
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Objective:To explore the relation of the radiochemical purity and in vivo imaging effect of 68Ga-1, 4, 7, 10-tetraazacyclododecane-1, 4, 7, 10-tetraacetic acid (DOTA)- D-phe1-Tyr3-Thr8-octreotide (TATE) injection. Methods:High performance liquid chromatography (HPLC) and thin-layer chromatography (TLC) methods were established to determine 68Ga-DOTATATE, 68Ga 3+ , 68Ga in colloidal form and 68Ga-DOTA- D-Phe1-Tyr3-Thr8-dethreonine-octreotide (heptapeptide) and to study the influence of precursor purity on radiochemical purity of labelled products. The uptake of 68Ga-DOTATATE injection with different radiochemical purities was investigated in nude mice bearing AR42J cells by microPET imaging and the tumor target/non-target (T/NT) value was calculated. One-way analysis of variance and Pearson correlation analysis were used to analyze the data. Results:The contents of 68Ga 3+ and 68Ga in colloidal form were not related with precursor purity ( r values: 0.385, 0.497, P values: 0.306, 0.137), while the content of 68Ga-DOTA-heptapeptide was positively related with the purity of DOTA-heptapeptide ( r=0.957, P<0.001). The radiochemical purities of 68Ga-DOTATATE injection were (87.0±2.3)%, (86.8±0.8)% and (94.0±3.1)% when the DOTATATE purities were 90.9%, 91.6% and 99.2%, respectively. The results of microPET imaging showed that the tumor uptake was positively related with the radiochemical purity of 68Ga-DOTATATE injection ( r=0.828, P<0.001), and the T/NT values of 68Ga-DOTATATE injection with radiochemical purities of 95.7%, 85.8%, 84.5% and 79.9% were 21.25±8.84, 8.50±1.51, 11.38±1.65 and 6.01±0.99, respectively ( F=11.48, P=0.001). Conclusion:The radiochemical purity of 68Ga-DOTATATE injection is impacted by the purity of labelled precursor and manufacturing processes and is related with the imaging effect in vivo.
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Objective To study the qualitative and quantitative standard of Shengui anti-pruritic mixture. Mehtods Sophorae Flavescentis Radix, Cnidii Fructus, Polygoni Multiflori Radix, Astragali Radix, Paeoniae Radix Alba and Glycyrrhizae Radix Et Rhizoma were identified by TLC.The contents of matrine and ferulic acid were determined by HPLC. Results The TLC showed the obvious characteristics with the spots clear and well-separated with no interference by negative control. Matrine showed a good linear relationship at 0.062 5- 2.500 0 μg (r=0.999 9) with a good meeting of adding sample recovery test. Ferulic acid showed a good linear relationship at 0.021 0-0.840 0 μg (r=0.999 9) with a good meeting of adding sample recovery test. Conclusions The method is easy-operated and accurate which showed a good specificity for the quality control of Shengui anti-pruritic mixture.
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Objective To establish a quality standard of yinqiao xiaozhen mixture. Methods Preparation of Forsyth-ia,Arctium lappa L.,and Honeysuckle were identified by TLC method.The concentration of baicalin in yinqiao xiaozhen mixture was determined by HPLC method. Results The qualitative identification method can detect Forsythia,Arctium lappa L.,and Honeysuckle.TLC spots were clear.TLC method has strong specificity.The linear range of baicalin was 0.122 5-1.531 2 μg,r=0.999 9,the average sample recovery rate was 99.42%,RSD was 2.19%,respectively. Conclusion The method is simple,ac-curate and repeatable,which can be used for quality control of Qinqiao xiaozhen mixture.
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Objective To establish a quality control method for bomeol and artificial musk in Xinfufang-Zhenzhusan and Xinfufang-Zhenzhugao.Methods We used petroleum ether-toluene-ethyl acetate (9:3:2)as developer for TLC to identify isoborneol and borneol and petroleum ether-dichloromethane (2:3) as developer for TLC to identificate musk ketone.Agilent 7890 B gas chromatograph,FDI detector;Column:Thermo-TG-WaxMS GC (0.25 mm × 30 m,0.25 mm) was employed;the carrier gas was high purity nitrogen and flow rate for 1 mg/ml,the injection port temperature is 200 C and detector temperature is 250 ℃;the split ratio is 10:1 and injection volume was 1 μl,using temperature programmed.Results The isoborneol,borneol and musk ketone in the range of 0.001-10 mg/ml showed good linearity.The recovery of the method is in the range of 95 ％ to 105 ％.The TLC for isobomeol,bomeol,musk ketone can be identified easily.Conclusions The method was simple and reasonable,which can be used for the quality control of borneol and artificial musk in the Xinfufang-Zhenzhusan and Xinfufang-Zhenzhugao.
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Objective To improve the quality standard ofKangjing pills.Methods The qualities of Angelica sinensis, Taxillus sutchuenensis, Radix paeoniae Alba, Eucommia ulmoides and Ligusticum chuanxiong Hort in the pills were identified by microscopic examination; the natures of Radix rehmanniae Praeparata, Radix paeoniae Rubra, Radix paeoniae Alba,Angelica sinensis and Ligusticum chuanxiong Hort were detected by thin layer chromatography (TLC); the content of Paeoniflorin were measured by high performance liquid chromatography (HPLC). The operating conditions by HPLC were InertSustain C18 (4.6 mm×250 mm, 5μm ), the mixture of acetonitrile-0.2% Phosphoric acid water (15:85) as mobile phase, 1.0 ml/min as flow speed and wavelength 316 nm.Results The results observed by microscopy were obvious; The results showed that the TLC spots of Radix rehmanniae Praeparata, Radix paeoniae Rubra, Radix paeoniae Alba, Angelica sinensis and Ligusticum chuanxiong Hort were fairly clear, and the according blank test showed no interference. Ferulic Acid showed a good linear relationship within the range of 0.067-0.168μg (r=0.9997) with an average recovery of 99.84% (RSD=1.22%). Conclusions Microscopy, TLC and HPLC are handy, safe and accurate forKangjing pills to determine the quality.
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Objective To establish a quality standard for Tibetan medicineRuyi-Zhenbao pill. Methods Thin-layer chromatography (TLC) was applied to identify 12 Tibetan medicinal materials, and High performance liquid chromatography (HPLC) was employed to determine the contents of gallic acid, dehydrodiisoeugenol, piperine, and cinnamaldehyde.Results The identified characteristics of TLC were distinct and the spots were clear. Linearity of gallic acid, dehydrodiisoeugenol, piperine, and cinnamaldehyde were in the range of 0.106-0.901μg, 0.033-0.281μg, 0.007-0.060μg, and 0.021-0.178μg, respectively. Average recovery was in the range of 98.47%-101.65% (RSD<3.0%).Conclusions The method of identification and content determination was good in terms of specificity, accuracy and repeatability, and can be used for quality control ofRuyi-Zhenbaopill.
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Objective To establish the quality control ofBaiduyin syrup.Methods The TLC was used to identity Radix paeoniae rubra, Radix Scutellariae. The quantitative determination of baicalin and buddleoside was completed by HPLC.Results The spots on TLC plates were distinct and high resolution. Compared with the negative samples, the contrast medicinal materials or control products showed that there were no spots of the same color in the corresponding position. The linear ranges of baicalin and buddleoside were 0.2179-2.1790 μg (r2=0.999 9), 0.1319-1.3190 μg (r2=0.999 7). TheRSD were 1.51% and 2.01%. Conclusions The established quality control method is simple, accurate and reproducible, which can be used for the quality control ofBaiduyin syrup.
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Objective To improve the quality standard of Baoyun pill. Methods The natures of Psoralea corylifolia, Radix Dipsaci and Loranthus parasiticus were detected by thin layer chromatography (TLC); the content of Hesperidine were measured by high performance liquid chromatography (HPLC). The operating conditions by HPLC were InertSustain C18 (4.6 mm×250 mm, 5 μm ), the mixture of methanol-acetic acid-water (35:4:61) as mobile phase, 1.0 ml/min as flow speed and wavelength 283 nm. Results The results showed that the TLC spots of Psoralea corylifolia, Radix Dipsaci and Loranthus parasiticus were fairly clear, and the according blank test showed no interference. Hesperidine showed a good linear relationship within the range of 0.820-4.920 μg(r=1.000 0)with an average recovery of 99.85%(RSD=0.21%).Conclusions The TLC and HPLC are handy,safe and accurate for Baoyun pills to determine the quality.
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Objective To improve the quality standard ofKangjing pills.Methods The qualities of Angelica sinensis, Taxillus sutchuenensis, Radix paeoniae Alba, Eucommia ulmoides and Ligusticum chuanxiong Hort in the pills were identified by microscopic examination; the natures of Radix rehmanniae Praeparata, Radix paeoniae Rubra, Radix paeoniae Alba,Angelica sinensis and Ligusticum chuanxiong Hort were detected by thin layer chromatography (TLC); the content of Paeoniflorin were measured by high performance liquid chromatography (HPLC). The operating conditions by HPLC were InertSustain C18 (4.6 mm×250 mm, 5μm ), the mixture of acetonitrile-0.2% Phosphoric acid water (15:85) as mobile phase, 1.0 ml/min as flow speed and wavelength 316 nm.Results The results observed by microscopy were obvious; The results showed that the TLC spots of Radix rehmanniae Praeparata, Radix paeoniae Rubra, Radix paeoniae Alba, Angelica sinensis and Ligusticum chuanxiong Hort were fairly clear, and the according blank test showed no interference. Ferulic Acid showed a good linear relationship within the range of 0.067-0.168μg (r=0.9997) with an average recovery of 99.84% (RSD=1.22%). Conclusions Microscopy, TLC and HPLC are handy, safe and accurate forKangjing pills to determine the quality.
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Objective To establish the quality standard for Haijinhuwei powder. Methods Corydalis Rhizoma, Angelicae Dahuricae Radix, Angelicae Sinensis Radix were identified by TLC. The content of tetrahydropalmatine was determined by HPLC. Results TLC spots were clear and specific.There was a good linear relationship between peak area and concentration of tetrahydropalmatine at the range of 10.78-107.8μg.mL-1(r=0.999 9).The average recovery rate was 96.57% and RSD was 1.40%(n=6). Conclusion All these results indicated that the developed TLC-HPLC method was proved to be reliable, accurate and specific, which could be used for the quality control of Haijinhuwei powder.
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Objective To establish the quality standard for Yanyan syrup. Methods Thin layer chromatography ( TLC) was used for the qualitative identification of Puerariae Lobatae Radix and Scrophulariae Radix. High performance liquid chromatography (HPLC) was used to determine the content of puerarin on Diamonsil C18(200 mm×4.6 mm,5μm) column with mobile phase consisting of methanol-0.5% acetic acid (25:75) at a flow rate of 1.0 mL?min-1.The detection wavelength was set at 250 nm. Results TLC spots were clear and well-separated without negative interference.The linear range of puerarin was 3-120μg?mL-1( r=0.999 7) with an average recovery of 97.44% ( RSD=2.07%,n=6) . Conclusion The method for quality and quantity of Yanyan syrup is simple, specific, accurate and reliable.It can be used for the quality control of Yanyan syrup.
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Objective This paper is intended for establishing quality standard of Ershiwuwei Shanhu pill. Methods The TLC was used to indentify Pyrethrum tatsienense, Sesami nigrum semen, Aquilariae lignum resinatum, Caryophmlli flos, Acori calami rhizoma, Chebulae fructus, Aucklandiae radix and Glycyrrhizae radix et rhizome. For hydroxysafflor yellow A, the HPLC system consisted of WondaSil-C18 (250 mm×4.6 mm, 5μm), methanol-acetonitrile- 0.7% phosphoric acid (26:2:72) as mobile phase, flow rate of 1.0 ml/min, detection wavelength at 403 nm. For liquiritin, the HPLC system consisted of WondaSil-C18 (250 mm×4.6 mm, 5μm), acetonitrile (A)-0.05% phosphoric acid (B) as mobile phase, flow rate of 1.0 ml/min, detection wavelength at 237 nm. And for crocin-I, the HPLC system consisted of WondaSil-C18 (250 mm×4.6 mm, 5μm), methanol-water (49:51) as mobile phase, flow rate of 1.0 ml/min, detection wavelength at 440 nm. Results The methods of TLC were simple with strong specificity and good reproducibility. The results of HPLC showed that calibration curve was linear in the ranges of 0.046 7-0.233 8μg for hydroxysafflor yellow A, and 0.510 6-1.531 8μg for liquiritin and 0.048 1-0.340 5μg for crocin-I. The average recovery rate was 102.01%, 99.50%and 99.32%, respectively. Conclusion The new method is more appropriate for the quality control of Ershiwuwei Shanhu pill.
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Objective To establish the quality standard ofQizhu-Fuzheng Yin, and to conduct a preliminary study on its stability.Methods Corydalis tuber and licorice were identified by TLC. The content of astragaloside was determined by UPLC-ELSD. The initial stability was studied by accelerated test method. Results The spots on TLC plates were clear without interference in the blank reference. The response of astragaloside was linear in the ranges of 36.5-365.0 μg/ml (r2=0.999 2), and the average recovery was 102.8 %, and theRSD was 2.4%. After 1, 2, 3, 6 months tests, the average contents of 3 batches astragaloside were 61.6, 60.4, 60.6μg/ml.ConclusionQizhu-Fuzheng Yin was simple preparation, quality control and stability.
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Objective To establish a method for quality control of xinshuaining mixture. Methods The herbal contents including red ginseng,milk veteh,root of red rooted salvia were identified by thin layer chromatography ( TLC) and the content of ginsenoside Rb1 in xinshuaining mixture was determined by high performance liquid chromatography ( HPLC ) . Results The herbs can be overtly identified by TLC. Ginsenoside Rb1 had a linear relationship in the range of 1. 095-5. 475μg, and the average recovery was 97. 3%(RSD 1. 98%). Conclusion The method is simple and rapid,and can be used for the quality control of xinshuaining mixture.
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Objective To establish the quality standard for mongolian medicine Rhaponticum uniflorum (L.) DC. with modern analysis methods. Methods Chlorogenic acid and apigenin were identified by thin -layer chromatography (TLC). The chlorogenic acid content was determined by high performance liquid chromatograghy ( HPLC). And HPLC was performed on Kromat Universil C18 ( 4.6 mm × 250 mm, 5 μm) with methanol-water-acetic acid ( v/v/v, 15:85:0.85) as mobile phase, the detection wavelength was 326 nm, the flow rate was 1.0 mL/min, and the column temperature was 20℃. Results The samples and the reference substance shared the same color spots at the same sites. The linear range of chlorogenic acid was 0.044 66-0.446 6μg (r=0.999 8), and the average recovery rate was 99.84%. Conclusion The method is simple, accurate, and with good reproducibility, and can be used for the quality control of Rhaponticum uniflorum ( L. ) DC.
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Objective To investigate and evaluate the quality of Cortex Ilicis Rotundae medicinal materials in Chinese herbal medicine market. Methods Twenty-two batches of Cortex Ilicis Rotundae commercial medicinal materials were identified and analyzed by characteristic identification, microscopic identification, thin layer chromatography ( TLC) and extractives determination, and the contents of syringin and pedunculoside were detected by high performance liquid chromatography (HPLC) according to the Chinese Pharmacopoeia published in 2010. And then the quality of the medicinal material of Cortex Ilicis Rotundae was evaluated comprehensively. Results Of the 22 batches of Cortex Ilicis Rotundae medicinal materials, 2 batches were adulterated with fake Cortex Ilicis Rotundae, one batch was inferior and was mixed with counterfeits, and the quality of 12 batches was also poor. Conclusion At present, the quality of Cortex Ilicis Rotundae medicinal materials in Chinese herbal medicine market varies greatly, and adulterants and the inferior are common.
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Objective To evaluate the quality of Radix et Caulis Ilicis Asprellae from Pingyuan planting base and Chinese herbal medicine market. Methods The water- and alcohol-soluble extracts from 19 batches of Radix et Caulis Ilicis Asprellae medicinal materials were detected according to Appendix ⅨH, ⅩA of the Chinese Pharmacopoeia ( 2010 edition). And the quality of the medicinal materials was evaluated by microscopic identification technology according to the method for Radix et Caulis Ilicis Asprellae recorded in Guangdong Provincial Chinese Medicine Standard, and then thin layer chromatography ( TLC) was optimized to establish the high performance liquid chromatography (HPLC) fingerprint. The HPLC was performed on Waters XBridgeTM C18 column (250 mm × 4.6 mm, 5μm) with acetonitrile(A)-0.2% (v/v) phosphorus acid (B) as the mobile phase by gradient elution, flow rate was 1.0 mL/min, and detection wavelength was 220 nm. Results The results of sample characters, TLC and microscopic identification showed that the samples of Radix et Caulis Ilicis Asprellae in Chinese herbal medicine markets were certified products, but stems and roots were blended. Seven common peaks were showed by HPLC and confirmed by similarity analytical software. The similarity of 15 batches of planting base samples was all above 0.9. Of 19 batches of the commercial samples, the similarity of 11 batches was above 0.9. The alcohol-soluble extract contents were in the range of 64.55 mg/g to 186.18 mg/g. Conclusion The medicinal materials of Radix et Caulis Ilicis Asprellae from Chinese herbal medicine market are certified products, but the qualities vary greatly for the blending of stems and roots and inadequate growth years. The quality of materials from planting base is better. The established method is helpful for the quality evaluation and control of Radix et Caulis Ilicis Asprellae.
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Objective To evaluate the quality of medicinal materials of Lignum Dalbergiae Odoriferae in Chinese herbal medicine market. Methods Eighteen batches of commercial medicinal materials of Lignum Dalbergiae Odoriferae were identified and analyzed by macroscopical identification, thin layer chromatography (TLC), and volatile oil assay according to the Chinese Pharmacopoeia published in 2010. Visible spectrometry was used to determine the content of total flavonoids from the qualified samples. And the gas chromatography was applied to evaluate the content of nerolidol from volatile oils of the qualified samples. Results Only 33.3%of the samples met the standard of Chinese Pharmacopoeia. The total flavonoid content of the qualified samples was in the range of 21.6-29.0 mg/g. The content of nerolidol from volatile oils of the qualified samples was in the range of 294-574 mg/g. Conclusion At present, the quality of medicinal materials of Lignum Dalbergiae Odoriferae in Chinese herbal medicine market and in clinic varies greatly, and adulterants and inferior are common. The contents of chemical components in different batches of samples are significant different.
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Objective To establish the quality standard of Radix Toddaliae Asiaticae. Methods Thin layer chromatography ( TLC) and high performance liquid chromatography ( HPLC) were used to identify and determine chloride nitidine and toddalolactone in Radix Toddaliae Asiaticae. The moisture and total ash contents were detected according to the methods recorded in appendix of Chinese Pharmacopeia (2010 edition) . Results Toddalolactone and chloride nitidine were detectable by TLC, the spots were clear and the dissociation was good. The established HPLC method was simple and accurate. The linear ranges of toddalolactone and chloride nitidine in Radix Toddaliae Asiaticae were 2.84~42.6 μg/mL and 25.6~385 μg/mL, and their recovery rates were 99.2 % ( RSD=1.12%) and 100 % ( RSD=0.71%) , respectively. The content of moisture was in the range of 75.8~98.9 mg/g and that of total ash was in the range of 12.4~33.6 mg/g. Conclusion The developed method is specific and accurate, and can provide useful reference for establishing quality standard of Radix Toddaliae Asiaticae.