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ObjectiveTo clarify the scientific validity of in vivo pharmacokinetic determination of the whole drug composition in Shenbai nanosuspension in rats， and to provide methodological guidance and theoretical basis for the in vivo study of multi-component complex system of traditional Chinese medicine（TCM） preparations. MethodThe concentration of the overall components， mainly total saponins and total polysaccharides in Shenbai decoction and Shenbai nanosuspension， was determined in rat plasma at different times by area under the absorbance-wavelength curve method（AUAWC）， and the concentration of individual ginsenoside Rg1 was determined by high performance liquid chromatography（HPLC）， and the methodology was verified. The pharmacokinetic parameters of the whole component were compared with those of ginsenoside Rg1 to evaluate the in vivo operational characteristics of the two preparations. ResultThe methodological investigations of AUAWC and HPLC were in accordance with the requirements. AUAWC analysis showed that the overall components in both the decoction group and the nanosuspension group showed a one-compartment model， with half-life（t1/2） of 2.43 h and 2.04 h， respectively. The relative bioavailability of Shenbai nanosuspension was 138.99%. HPLC assay showed that ginsenoside Rg1 in the decoction group and the nanosuspension group showed a two-compartment model， with distribution half-life（t1/2α） of 0.13 h and 2.55 h， and elimination half-life（t1/2β） were 14.28 h and 3.85 h， respectively. The relative bioavailability of Shenbai nanosuspension was 127.49%. Compared with Shenbai decoction， the time to peak（tmax）， peak concentration（Cmax） and area under the drug-time curve（AUC） of the overall components and ginsenoside Rg1 in Shenbai nanosuspension were increased. ConclusionThe established AUAWC can be used for the pharmacokinetic study of the overall components of TCM preparations， which is complementary to the results of individual components measured by HPLC， and can provide useful reference for the in vivo study of new dosage forms of TCM.
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Purpose: To compare the retinal sensitivities between the blue?on?yellow perimetry (BYP)/short?wavelength automated perimetry (SWAP) and green?on?yellow perimetry (GYP) among patients with and without nuclear sclerosis among glaucoma suspects. Methods: After ophthalmic examination, patients were subjected to two perimetric tests: BYP and GYP. The visual field (VF) parameters were compared between the two perimeters (p < 0.05 was considered significant). Results: Fifty?five eyes of 39 patients with a mean age of 60.53 ± 9.70 years were included in the study. Twenty?one eyes had clear lens or pseudophakia. Twenty?six eyes had lower grades of nuclear sclerosis (NO2NC2, NO3NC3) and eight eyes had higher grades of cataract (NO4NC4, NO5NC5). The mean retinal sensitivity (RS) in BYP was 22.08 ± 5.02 (dB) and in GYP was 23.84 ± 5.50 (dB) (p = 0.08). The mean defect in BYP was ?2.56 ± 4.40 (dB) and in GYP was ?3.24 ± 5.05 (dB), pattern standard deviation (PSD) in BYP was 3.65 ± 1.91 (dB) and in GYP was 3.83 ± 1.99 (dB), and foveal threshold (FT) was 24.20 ± 4.32 (dB) in BYP and 28.10 ± 4.50 (dB) in GYP. The two perimeters showed good agreement by the Bland–Altman plot for all parameters. Fourteen eyes showed perimetric changes suggestive of glaucoma by BYP. In these, GYP had a sensitivity of 92.86% (95% CI of 66.13% to 99.82%) and specificity of 95.12% (95% CI of 83.47% to 99.40%). Conclusion: BYP and GYP show good agreement. They are comparable in clear media as well as in different grades of nuclear sclerosis. GYP showed good sensitivity and specificity compared to BYP.
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Objective:To evaluate the clinical efficacy of 1 064 nm/755 nm dual wavelength laser on hair removal.Methods:A total of 60 patients aged 18-52 (30±7) years in our hospital from January 2017 to December 2017 were collected. 1 064 nm and 755 nm laser hair removal was performed at the same symmetrical areas or two different areas in the same patient. We performed 6 sessions of laser treatment at 6-week intervals and the effect was evaluated 6 weeks after the last session.Results:The hair removal efficacy was 96.7% (58 cases) at 1 064 nm, 96.7% (58 cases) at 755 nm laser treatment. There was no significant difference in the effective rate between two wavelengths laser hair removal methods ( P>0.05). The incidence of pigmentation was 1.7% (1 case) at 1 064 nm laser and was 3.3% (2 cases) at 755 nm laser without significant difference ( P>0.05). No hypopigmentation, blister or scar appeared in all patients. The total satisfactory rate was 95.0% (57 cases) at 1 064 nm, 98.3% (59 cases) at 755 nm laser treatment, respectively. Conclusions:1 064 nm/755 nm dual wavelength laser has definite therapeutic effect and safety on hair removal.
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Objective To establish a high performance liquid chromatography(HPLC) method for simultaneous determination of the contents of 7 components of chlorogenic acid, caffeic acid, paeoniflorin, ammonium glycyrrhizinate, baicalin, baicalein, and wogonin in Piqin oral liquid. Methods A double-wavelength HPLC method was performed. The column was Agilent Zorbax SB-C18 (250 mm × 4.6 mm, 5 μm). The mobile phase was 0.02% phosphoric acid aqueous solution (A)-acetonitrile (B) gradient elution; Flow rate: 1.0 ml/min; Column temperature: 35℃; Injection volume: 20 μl; Detection wavelength: 0-18.0 min, 325 nm (detect chlorogenic acid, caffeic acid); 18.0-65.0 min, 280 nm (detect paeoniflorin, baicalin, baicalein, ammonium glycyrrhizinate, wogonin). Results The chlorogenic acid, caffeic acid, paeoniflorin, ammonium glycyrrhizinate, baicalin, baicalein and wogonin were completely separated. Seven components have a good linear relationship between the peak area and concentration, with the recoveries between 96.41% and 99.70%. Conclusion This method is simple, accurate and reproducible, and can be used for the quality control of Piqin oral liquid.
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OBJECTIVE：To develop a method for simultaneous determination of 5 components in classical formula Huaihua san，including rutin ，naringin，neohesperidin，quercetin and pulegone. METHODS ：HPLC wavelength switching method was adopted. The determination was performed on Cosmosil C 18 column with mobile phase consisted of acetonitrile- 0.05％ phosphoric acid solution （gradient elution ）at the flow rate of 1.0 mL/min. The detection wavelengths were set at 257 nm for rutin ，283 nm for naringin and neohesperidin ，254 nm for quercetin ，252 nm for pulegone ，respectively. The column temperature was set at 30 ℃， and sample size was 10 μL. RESULTS：The linear range was 21.7-2 170 μg/mL for rutin，46-4 600 μg/mL for naringin，22.3- 2 230 μg/mL for neohesperidin，0.96-96 μg/mL for quercetin，2.7-270 μg/mL for pulegone（all r＞0.999），respectively. RSDs of precision，stability（24 h）and reproducibility tests were all lower than 2％（n＝6）. Average recoveries were 100.70％，99.31％， 101.10％，100.03％ and 99.63％（all RSD ＜2％，n＝9）. Among 3 batches of Huaihua san samples ，the contents of above 5 components were 20.055-22.615，25.557-27.806，11.428-13.250，0.350-0.478，2.372-4.011 mg/g，respectively. CONCLUSIONS ： Established method is simple ，accurate and reproducible ，and could be used for the simultaneous determination of 5 components in Huaihua san.
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The use of non-invasive blood glucose detection techniques can help diabetic patients to alleviate the pain of intrusive detection, reduce the cost of detection, and achieve real-time monitoring and effective control of blood glucose. Given the existing limitations of the minimally invasive or invasive blood glucose detection methods, such as low detection accuracy, high cost and complex operation, and the laser source's wavelength and cost, this paper, based on the non-invasive blood glucose detector developed by the research group, designs a non-invasive blood glucose detection method. It is founded on dual-wavelength near-infrared light diffuse reflection by using the 1 550 nm near-infrared light as measuring light to collect blood glucose information and the 1 310 nm near-infrared light as reference light to remove the effects of water molecules in the blood. Fourteen volunteers were recruited for
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Humans , Blood Glucose , Diabetes Mellitus , Nonlinear DynamicsABSTRACT
OBJECTIVE：To establish a method for simultaneous determination of 12 components including naringin ， hesperidin，neohesperidin，aloe emodin ，rhein，notopterol，emodin，honokiol，isoimperatorin，magnolol，chrysophanol and physcion in classical formula Sanhua tang. METHODS ： HPLC-multi-wavelength switching technology was adopted. The determination was performed on COSMOSIL C 18 with mobile phase consisted of acetonitrile- 0.1％ phosphoric acid （gradient elution）at the flow rate of 1.0 mL/min. The detection wavelength was 280 nm（naringin，hesperidin，neohesperidin），254 nm （aloe emodin ，rhein，chrysophanol，emodin methyl ether ），310 nm（notopterol，emodin，honokiol，isoimperatorin，magnolol）. The column temperature was set at 30 ℃，and the sample size was 10 μL. RESULTS：A total of 12 components were well separated without negative interference. The linear range of naringin ，hesperidin，neohesperidin，aloe emodin ，rhein，notopterol， emodin，honokiol，isoimperatorin，magnolol，chrysophanol and physcion were 55.4-5 540，3.8-380，45.6-4 560，1.2-120， 2.1-210，2.2-220，2-200，2.4-240，0.8-80，1.2-120，1.7-170，1.1-110 μg/mL（R 2≥0.999 6），respectively. The detection limits were 0.064，0.024，0.053，0.018，0.020，0.041，0.050，0.091，0.030，0.180，0.028 and 0.083 μg/mL，respectively. The limits of quantitation were 0.213，0.075，0.174，0.060，0.063，0.138， 0.166，0.323，0.130，0.600，0.094 and 0.275 μ g/mL，respec- 9721004） tively. RSDs of precision ，stability （24 h） and repeatability 2633531778@qq.com tests were all lower than 2％（n＝6）. Average recoveries were 99.54％，99.69％，100.01％，99.93％，100.36％，99.65％， 100.03％，100.47％，99.97％，100.68％，99.90％，100.17％ （all RSDs were lower than 2％，n＝6），respectively. CONCLUSIONS ：Established HPLC-multi- wavelength switching technology is simple ，specific and stable ，which could be used for the simultaneous determination of 12 components in Sanhua tang as naringin，hesperidin，neohesperidin.
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The resonance light scattering (RLS) spectral characteristics of the interaction between rose Bengal and mexiletine hydrochloride in the presence of cetylpyridinium bromide were investigated. A dual-wavelength resonance light scattering (DWO-RLS) method for the determination of mexiletine hydrochloride in drugs was established. In a weakly acidic solution, rose Bengal interacts with mexiletine hydrochloride and cetylpyridinium bromide to form a red ternary ion association complex, which led to a significantly enhanced resonance light scattering signal and produced two strong characteristic scattering peaks at 372 nm and 596 nm. In these two wavelengths the mass concentration of mexiletine hydrochloride was in the range of 0.004 to 0.65 mg·L-1 and had a good linear relationship with the resonance light scattering enhancement intensity (ΔIRLS), with detection limits of 0.003 2 mg·L-1 (372 nm) and 0.003 8 mg·L-1 (596 nm), respectively. When measured by the dual-wavelength resonance light scattering (DWO-RLS) technique, the detection limit was lower, only 0.001 8 mg·L-1. When the DWO-RLS method was applied to the determination of mexiletine hydrochloride in commercially available mexiletine hydrochloride tablets, and the recovery was 98.5%-103%, and the relative standard deviation was 2.0%-2.7%.
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Objective::To develop high performance liquid chromatography-diode array detector (HPLC-DAD) wavelength switching for simultaneously determining the contents of inosine, loganic acid, chlorogenic acid, amygdalin, hydroxysafflor yellow A, gentiopicroside, ferulic acid and liquiritin in 15 batches of material benchmarks of Shentong Zhuyutang. Method::The quantitative analysis was carried out on a Thermo Hypersil GOLD C18 column (4.6 mm×250 mm, 5 μm) with mobile phase of acetonitrile-0.1%phosphoric acid aqueous solution for gradient elution, the flow rate was 1.0 mL·min-1, the detection wavelengths were set as 248 nm (0-11 min, inosine), 235 nm (11-14 min, loganic acid), 324 nm (14-16 min, chlorogenic acid), 220 nm (16-19 min, amygdalin and hydroxysafflor yellow A), 274 nm (19-26 min, gentiopicroside), 247 nm (26-54 min, ferulic acid and liquiritin), the column temperature was maintained at 25 ℃. According to the contents of eight active components in 15 batches of material benchmarks, orthogonal partial least squares discriminant analysis (OPLS-DA) in SIMCA 14.1 was used to evaluate the quality difference of each batch of samples. Result::Each component had good separations, the linear ranges of the above 8 components were 2.1-67.2, 1.812 5-58, 1.937 5-62, 5.212 5-166.8, 8.45-270.4, 7.075-226.4, 1.775-56.8, 3.875-124 mg·L-1, respectively (r≥0.999 6). The average recoveries of them were 99.23%, 100.09%, 99.33%, 98.85%, 99.15%, 98.75%, 99.42%, 98.96%, respectively (RSD<2%). The contents of the above eight components in 15 batches of material benchmarks were 0.183 5-0.250 3, 0.173 1-0.265 3, 0.069 5-0.169 8, 0.959 2-1.458 2, 1.905 4-2.553 3, 0.933 3-1.997 5, 0.084 6-0.143 4, 0.212 5-0.704 3 mg·g-1, respectively. Liquiritin, ferulic acid, gentiopicroside and hydroxysafflor yellow A were determined to have significant impact on the quality of different batches of material benchmarks of Shentong Zhuyutang through OPLS-DA. Conclusion::The established method for simultaneous determination of multi-components is reliable, simple and in line with the requirements of methodological verification. It is suitable for the quality control of research and development of compound preparations of Shentong Zhuyutang.
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@#To establish HPLC dual-wavelength fingerprint of Artemisia rupestris L. , and provide a scientific basis for the improvement of its quality specifications. The separation was performed on an Agilent Zorbax SB-C18(4. 6 mm×250 mm, 5 μm)column maintained at 32 ℃, with methanol-0. 2% formic acid-water gradient elution at flow rate of 1. 0 mL/min and the UV detection wavelength at both 245 and 325 nm. The sample injection volume was 20 μL. The fingerprint of Artemisia rupestris L. was established. 7 and 8 common peaks were found, respectively, of which 5 common peaks were identified, and the similarity among 9 batches of Artemisia rupestris L. and the fingerprints of control was over 0. 9. The HPLC dual-wavelength fingerprint of Artemisia rupestris L. was established for the first time, providing a new scientific basis for its identification and quality control.
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OBJECTIVE: To establish the HPLC fingerprint of Valeriana jatamansi and provide a reference for its effective quality control. METHODS: The HPLC-DAD analysis was performed on Diamonsil C18 column (4.6 mm×250 mm, 5 μm), with acetonitrile (A)-0.1% formic acid (B) solution as the mobile phase for gradient elution, the detection wavelength was set at 327 nm (0-33 min) and 256 nm (33-90 min), the flow rate was 1.0 mL•min-1, and the column temperature was maintained at 30 ℃. The fingerprints of 25 batches of Valeriana jatamansi samples were analyzed by similarity analysis, hierarchical clustering analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares discriminant analysis (PLS-DA). RESULTS: The fingerprints of 25 batches of Valeriana jatamansi samples were established. There were 36 common peaks in the fingerprints and nine common peaks were identified by reference substances. The fingerprints similarity of 18 batches of samples was over 0.9, and the samples were classified into two groups. Six components were the main markers that cause differences in different batches of samples, including valepotriate, acevaltrate, isochlorogenic acid A, and some others. CONCLUSION: HPLC fingerprint combined with recognition of chemical pattern can reflect the intrinsic quality of Valeriana jatamansi, which may provide reference for the quality control and evaluation of Valeriana jatamansi.
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OBJECTIVE: To establish an HPLC method for simultaneous determination of nine components, i.e., paeoniflorin, naringin, hesperidin, neohesperidin, paeonol, asperosaponin , glycyrrhizic acid, curcumin and acetyl-11-keto-beta-boswellic acid, and evaluate the overall quality of Dieda pills. METHODS: The analysis was performed on an Agilent 1260 Infinity LC System with a diode array detector. The chromatographic separation was performed on Agilent Poroshell 120 EC-C18 (4.6 mm×100 mm, 2.7 μm) column. The mobile phase was a mixture of acetonitrile (mobile phase A) and water containing 0.1% phosphoric acid aqueous solution (mobile phase B). The gradient elution program was as follows: 5%-18%A for 0-7 min, keeping 18%A for 7-15 min, 18%-35%A for 15-27 min, 35%-60%A for 27-32 min, 60%-95%A for 32-42 min, keeping 95%A for 42-45 min.The flow rate was set at 1.0 mL•min-1, the column temperature was maintained at 30 ℃ and the injection volume was 5 μL. The detection wavelength was set at 230 nm for paeoniflorin, 283 nm for naringin, hesperidin and neohesperidin, 274 nm for paeonol, 212 nm for asperosaponin , 251 nm for glycyrrhizic acid, 440 nm for curcumin and 251 nm for acetyl-11-keto-beta-boswellic acid, respectively. RESULTS: All the nine components achieved good separation.The linear ranges fell with in the range of 0.1-1.0 μg for paeoniflorin, naringin, neohesperidin andacetyl-11-keto-beta-boswellic acid, 0.2-2.0 μg for hesperidin and asperosaponin , 0.04-0.4 μg for paeonol, 0.02-0.2 μg for glycyrrhizic acid and 0.01-0.1 μg for curcumin,respectively(r2≥0.999 8). The average recoveries (n=6) were 96.95%-100.4% and the RSDs were 0.21%-0.81%. CONCLUSION: The developed method is simple, accurate, reliable, and can be used for the overall quality control and quality evaluation of Dieda pills.
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Objective: To establish an HPLC method for the simultaneous content determination of seven constituents in Compound Yi’anning Pills (CYP). Methods: The determination was performed on Shim-pack GIST C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid (gradient elution: 0-5 min, 5% acetonitrile; 5-12 min, 5%-12% acetonitrile; 12-17 min, 12%-20% acetonitrile; 17-30 min, 20% acetonitrile; 30-36 min, 20%-50% acetonitrile; 36-45 min, 50%-80% acetonitrile; 45-70 min, 80% acetonitrile) at the flow rate of 1.0 mL/min. The detection wavelength was set at 203 nm for notoginsenoside R1, ginsenoside Rg1, and ginsenoside Rb1, 220 nm for schisantherrin A, 250 nm for schisandrin, 268 nm for salvianolic acid B, and 270 nm for tanshinone IIA. The column temperature was set at 35 ℃ and the injection volume was 10 μL. Results: The linear range of detection concentration was 0.015-0.150 mg/mL for notoginsenoside R1, 0.077-0.766 mg/mL for schisandrin, 0.006-0.062 mg/mL for salvianolic acid B, 0.009-0.092 mg/mL for buddleodide, 0.050-0.503 mg/mL for ginsenoside Rg1, 0.067-0.670 mg/mL for ginsenoside Rb1, and 0.011-0.108 mg/mL for tanshinone IIA. Average recoveries respectively were 99.5%, 99.8%, 99.2%, 98.9%, 96.9%, 98.8%, and 97.1%. Conclusion: The method is simple, effective, and accurate, which can be used for simultaneous determination of seven active constituents in CYP.
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Objective: To establish an HPLC wavelength switching method for the simultaneous content determi- nation of verbascoside,paederosidic acid methyl ester,asperulosidic acid,asperuloside,calycosin7-O-β-D-glucopyran- oside,ononin,calycosin,formononetin and batatasinin Shenkangling granules(Radix Rehmanniae,Herba Hedyotis Diffusae,Radix Astragali,Rhizoma Dioscoreae,etc.). Methods: The Shenkangling granules were extracted with 50% aqueous methanol to prepare the test solution. The HPLC analysis was performed on thermostatic Agilent Eclipse XDB-C18 (250 mm×4.6 mm,5 μm)a 30℃,with the mobile phase consisting of acetonitrile-0.2% phosphoric acid solution at 0.9 ml/min flow rate in a gradient elution manner,and the detection wavelength was set at 334,238,254 and 270 nm, respectively. Results The above mentioned nine compounds showed good linearity in turn within the range of 3.09- 61.80,3.67-73.40,1.98-39.60,2.51-50.20,1.39-27.80,1.06-21.20,0.87-17.40,2.79-55.80,and 2.16-43.20 μg/ml, respectively,and their average recovery was 99.34%,100.03%,97.67%,98.63%,97.96%,96.93%,97.48%,99.87%, and 98.95% with the RSD of 0.88%,1.15%,1.28%,1.49%,0.99%,1.41%,1.37%,0.72%,and 1.25%,respectively.Conclusion: The method is easy to operate,repeatable,and can be used for quality control of Shenkangling granules.
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Objective: To establish a simple,rapid and novel Rayleigh light scattering(RLS)method for rapid determination of mexiletine hydrochloride in drugs. Methods: In the presence of acid Tris-HCl medium and cetylpyri- dinium bromide,eosin Y reacted with mexiletine hydrochloride to form a ternary ion association complex with two charac- teristic scattering peaks by electrostatic attraction. The detection wavelengths were 368 and 586 nm. There was a linear relationship between the mexiletine hydrochloride concentration in a certain range and the Rayleigh light scattering en- hancement intensity(ΔIRLS)of the association complex. Single-wavelength Rayleigh scattering(SWO-RLS)method or dualwavelength Rayleigh light scattering(DWO-RLS)method was used to determine the content of mexiletine hydrochloride, and the mexiletine hydrochloride content was calculated according to the regression equation of standard curve. Results: The linear ranges of mexiletine hydrochloride were 0.005-0.65 mg/L(SWO-RLS method,368 nm),0.004-0.65 mg/L (SWO-RLS method,586 nm)and 0.004-0.65 mg/L(DWO-RLS method,368 nm+586 nm),respectisely. Detection lim- its were 0.0033(SWO-RLS method,368 nm),0.0040(SWO-RLS method,586 nm)and 0.0018 mg/L(DWO-RLS method, 368 nm+586 nm),respectisely. The recovery and relative standard deviation(RSD,n=5)for a SWO-RLS method were 98.6-103% and 1.4-1.8%,respectively(SWO-RLS method,368 nm). Conclusion: The method is simple,rapid, highly sensitive and high selectie.
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OBJECTIVE： To develop a method for simultaneous determination of 7 components of Niuhuang qingwei pills as chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol. METHODS： HPLC-wavelength switching method was adopted. The determination was performed on Agilent ZORBAX SB-C18 column with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid （B） gradient elution at the flow rate of 1.0 mL/min. The detection wavelengths were set at 348 nm （chlorogenic acid）， 238 nm （geniposide）， 330 nm （forsythoside A）， 280 nm （narirutin and baicalin）， 237 nm （ammonium glycyrrhetate）， 254 nm （chrysophanol）. The column temperature was 30 ℃， and sample size was 10 μL. RESULTS： The linear ranges of chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol were 0.011 67-0.233 4 μg （r＝0.999 4）， 0.042 91-0.858 1 μg （r＝0.999 4）， 0.125 0-2.500 μg （r＝0.999 9）， 0.118 0- 2.360 μg （r＝0.999 9）， 0.119 6-2.392 μg （r＝0.999 7）， 0.030 57-0.611 4 μg （r＝0.999 6）， 0.006 201-0.124 0 μg（r＝0.999 4）， respectively； the limits of quantitation were 1.167， 0.858， 1.250， 1.180， 1.196， 0.611， 0.620 μg/mL， respectively； RSDs of precision tests were 0.98％， 1.04％， 0.59％， 1.50％， 0.83％， 1.24％ and 1.32％ （n＝6）， respectively. RSDs of stability tests were 1.21％， 0.97％， 1.42％， 0.71％， 0.98％， 1.87％ and 1.63％ （n＝6， 12 h）， respectively. Average recoveries were 98.32％， 98.11％， 98.81％， 98.50％， 98.30％， 98.16％ and 97.83％， and the RSDs were 1.37％， 1.41％， 0.64％， 1.01％， 1.18％， 1.16％ and 1.16％ （n＝6）， respectively. CONCLUSIONS： Established method is easy and reproducible. It can be used for the quality control of Niuhuang qingwei pills.
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OBJECTIVE： To develop an method for determining the contents of dehydrocorydine and salvianolic acid B in Shuangshen tongguan capsules simultaneously. METHODS： The HPLC-dual wavelength switching method was used. The determination was performed on Waters symmetry C18 column with mobile phase consisted of acetonitrile-0.05％ phosphoric acid solution （gradient elution） at the flow rate of 1.0 mL/min， the detection wavelength was 286 nm （salvianolic acid B） and 336 nm （dehydrocorydine）. The column temperature was maintained at 25 ℃， and sample size was 10 μL. RESULTS： Under this condition， dehydrocorydaline and salvianolic acid B could be separated in baseline. The linear range of them were 0.157-1.259 μg and 0.391-3.131 μg （r＝0.999 9）. RSDs of precision， reproducibility and stability tests （within 24 h） were all lower than 2.00％ （n＝6-10）. The average recovery rates were 101.61％ and 102.85％ （RSD＝3.59％ and 2.85％， n＝6）. CONCLUSIONS： Established HPLC-dual wavelength switching method can be used for simultaneous determination of dehydrocorydine and salvianolic acid B in Shuangshen tongguan capsules. The method is simple and rapid， and can be used for the quality control of Shuangshen tongguan capsule.
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OBJECTIVE： To establish a method for quality control of Peony pollen buccal tablets， and to provide reference for the formulation of quality standard. METHODS： TLC method was used for qualitative identification of paeoniflorin， kaempferol and luteolin in Peony pollen buccal tablets according to 2015 edition of Chinese Pharmacopeia （part Ⅳ）. The contents of paeoniflorin and oxypaeoniflorin in Peony pollen buccal tablets were determined by dual-wavelength HPLC method [The determination was perform on Agilent TC-C18 column with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid solution （B） with gradient elution at the flow rate of 1.0 mL/min. The detection wavelength was set at 230 nm for paeoniflorin and 258 nm for oxypaeoniflorin. Sample size was 20 μL]. RESULTS： TLC identification of paeoniflorin， kaempferol and luteolin showed that the same color characteristic spots of control chromatogram appeared in the corresponding positions of sample chromatogram without interference from negative samples. The linear range of paeoniflorin and oxypaeoniflorin were 7.2-86.4 μg/mL and 2.72-32.64 μg/mL（r≥0.999 7），respectively. The average recoveries were 99.12％ and 98.65％， and RSD were 1.54％ and 2.53％（n＝6），respectively. RSDs of precision （n＝6）， stability （n＝8） and reproducibility （n＝6） tests were all lower than 3.0％. CONCLUSIONS： The method is simple and reproducible， and can be used for quality control of Peony pollen buccal tablets.
ABSTRACT
In order to evaluate the quality of Styrax more comprehensively,this study attempted to establish an HPLC wavelength switching method to simultaneously determine the content of seven compounds in Styrax,and chemometrics were used to analyze the quality difference between different sources of Styrax,and finally establish a characteristic chromatogram of Styrax. The column was Agilent ZORBAX Extend C18( 4. 6 mm×250 mm,5 μm) with phase a mixture of acetonitrile-0. 1% phosphoric acid aqueous solution as the mobile phase in a gradient elution procedure; the detection wavelength was set as follows: 0-13. 5 min,194 nm( benzoic acid);13. 5-20. 5 min,278 nm( cinnamic acid); 20. 5-32 min,194 nm( benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid); 32-55 min,241 nm( abietic acid). The methodological verification results showed that when the injection masses of benzoic acid,cinnamic acid,benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid and abietic acid were0. 006 948-0. 694 8,0. 001 426-0. 142 6,0. 013 16-0. 658 0,0. 006 148-0. 614 8,0. 008 035-0. 803 5,0. 002 121-0. 212 1,and0. 010 172-1. 017 2 μg,respectively,there were good linear relationship between injection mass and peak area. The average recovery rates of seven compounds were in the range from 94. 34% to 105. 8%,and all RSD were less than 3. 0%( n = 6). The methodological verification results showed that the developed HPLC wavelength switching method has good accuracy and repeatability. The results of the sample analysis showed that the quality of Styrax from different sources was quite different. The chromatogram of Styrax reference material( S1) was used as the reference chromatogram to calculate the fingerprint similarity of each batch of samples. The results showed that the similarities of samples S2-S10 were 0. 952,0. 949,0. 981,0. 351,0. 751,0. 969,0. 979,0. 992 and 0. 971,respectively.The similarity values of other batches samples were satisfactory,except for sample S5 and S6,indicating that the quality difference among these samples is small. The similarity values of S11-S20 were 0. 060,0. 055,0. 054,0. 285,0. 092,0. 002,0. 044,0. 044,0. 044,and 0. 040,respectively. The results showed that compared with the sample S1,there was a large quality difference among S11-S20. Based on the chromatograms of S1-S10,the HPLC characteristic chromatograms of Styrax was established and the purpose is to give reference to other pharmaceutical researchers. The newly developed HPLC wavelength switching method have the advantages of simplicity,reproducibility and specificity,and the developed HPLC characteristic chromatograms provided a reference method for the overall quality evaluation of Styrax.
Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Phytochemicals , Quality Control , Reproducibility of Results , Styrax , ChemistryABSTRACT
Malignant tumor is one of the most deadly diseases in the world. Researches focus on finding tumor therapy with better therapeutic efficiency and fewer side effects. Improving the therapeutic effect and reducing the side effects are the two hot topics in the field of malignant tumors treatment. As one of the new methods for non-invasive treatment of malignant tumors, photodynamic therapy (PDT) has the advantage of low cytoxicity and low drug resistance. PDT induces reactive oxygen species (ROS) production by irradiating light to specific sites, causing tumor cell apoptosis and necrosis, and achieving therapeutic purposes. Compared with the traditional PDT, long-wavelength light-triggered photodynamic therapy has deep tissue penetration and less cytoxicity. In this paper, the technical development of the long-wavelength light-triggered PDT was summarized including photosensitizers, two-photon activated PDT and upconversion PDT. The research progress of this therapeutic method in the treatment of malignant tumors was also reviewed.