1.Determination of Enantiomer in Rivaroxaban by HPLC
Qianru ZHANG ; Qi ZHANG ; Xiaofeng GUO ; Wenmin GUO
China Pharmacist 2014;(10):1629-1631
Objective:To establish a method for the determination of enantiomer in rivaroxaban by HPLC. Methods:A Chiralpak IA column (250 mm × 4. 6 mm, 5 μm) was used with the mobile phase of 100% methanol. The flow rate was 1. 0 ml·min-1 . The detection wavelength was set at 250 nm and the column temperature was 40℃. Results:The resolution of rivaroxaban and the enanti-omer was above 2. 0. The linear range of them was 0. 5-1 000. 00 μg·ml-1(r=0. 999 9). The detection limit of the enantiomer was 0. 17ng and the average recovery was 102. 9% with RSD of 1. 54%(n=6). Conclusion:The method is accurate and rapid, and suit-able for the determination of the enantiomer in rivaroxaban.
2.Mechanisms of curcumin protecting endothelial cells against ischemia and reperfusion injury
Wenmin HUA ; Zhongqin LIANG ; Yun FANG ; Zhenlun GU ; Ciyi GUO
Chinese Pharmacological Bulletin 2003;0(08):-
Aim To investigate the mechanisms in protecting HUVEC against ischemia/reperfusion(I/R) injury directed by curcumin.Methods Hypoxia/reoxgenation(H/R) model was established on HUVEC.MTT colorimetric assay was used to observe the injury degree of hypoxia and reoxygenation at the different time.With preconditioning by different concentration of Cur,the survival rate of HUVEC subjected to H/R was assessed by MTT colorimetric assay.Pretreated with Cur(5 ?mol?L-1),the expression of LC3,cathepsin B,cathepsin L,Bax and Bcl-2 were observed by fluorescent staining and Western blot in HUVEC during H/R process.Results Cur(1.25~5 ?mol?L-1) played a protective role during H/R in HUVEC in a dose-dependent manner.During H/R,the expressions of LC3,cathepsin B and the ratio of Bax/Bcl-2 increased,and the nuclear translocation of cathepsin L was induced;when cur was pretreated,LC3 was furtherstrengthened,at the same time,the up-regulation of cathepsin B,the ratio of Bax/Bcl-2 and the nuclei-location of cathepsin L were inhibited partly by Cur.Conclusions Cur can raise the survival rate of HUVEC in the process of H/R.Cur increases the autophagy activity,depresses cathepsins and Bax/Bcl-2 to protect the endothelial cells.
3.Determination of Optical Isomers in Bortezomib by HPLC
Na LIU ; Haixia LI ; Xiaoxue BAI ; Wenmin GUO
China Pharmacist 2017;20(1):156-158
Objective:To establish a method for the determination of three optical isomers in bortezomib. Methods: An HPLC method was used with a ChiralPAKAY-H normal phase chiral column (250 mm × 4. 6 mm, 5 μm). The mobile phase was n-hexane-ethanol-methanol-trifluoroaceticacid (90 ∶7. 5∶2. 5∶0. 1) and the flow rate was 0. 8 ml·min-1 . The detection wavelength was set at 270 nm. The column temperature was 40℃ and the injection volume was 5 μl. Results: The separation of bortezomib from the three optical isomers was more than 2. 0. The linear range of the three optical isomers was 0. 6-20μg·ml-1(r≥0. 999 7). The average re-covery was 104. 1%, 105. 5% and 92. 0% with RSD of 2. 3%, 2. 4% and 2. 7%, respectively (n=9). The limit of quantification and detection limit was 3 ng and 1 ng, respectively. Conclusion:The method is rapid and accurate, and can be used for the determi-nation of optical isomers in bortezomib.
4.Determination of Carfilzomib for Injection by HPLC
Na LIU ; Yanjiao WANG ; Haixia LI ; Wenmin GUO
China Pharmacist 2016;19(10):1959-1960
Objective:To establish an HPLC method to determine the content of carfilzomib for injection. Methods:The chroma-tographic column was a Waters symmetry C18(250 mm ×4.6 mm, 5 μm)column, the sample solvent was methanol, the mobile phase was 0. 05% trifluoroacetic acid-acetonitrile(57 ∶43) at a flow rate of 1. 0 ml · min-1 , the detection wavelength was 210 nm, the col-umn temperature was 25℃ and the injection volume was 10 ml. Results:The linear range of carfilzomib was 120-600 μg·ml-1 ( r=0. 999 7). The average recovery was 100. 4%( RSD=0. 24%,n=9). Conclusion:The method is rapid and effective, which can be used for the content determination of carfilzomib for injection.
5.Determination of the Enantiomer in Safinamide Mesilate by HPLC
Qi ZHANG ; Qianru ZHANG ; Jingyuan LIU ; Wenmin GUO
China Pharmacist 2016;19(3):582-584
Objective: To establish a determination method for the enantiomer in safinamide mesilate. Methods: A Chiralpak ASH (250 mm ×4. 6 mm, 5 μm) column was used with the mobile phase of n-hexane-ethanol-diethylamine (75 ∶ 25 ∶ 0. 1). The flow rate was 1. 0 ml·min-1 . The wavelength was set at 225 nm. The column temperature was 35℃. Results: The resolution of safinamide mesilate and the enantiomer was above 2. 0. The linear range of them was 1. 007-2 517. 500 μg·ml-1 and 0. 909-2273. 200 μg·ml-1 ,respectively(r = 0. 999 0). The average recovery of the enantionmer was 104. 9% with RSD of 2. 3% (n = 9). Conclusion: The method is accurate and rapid, and suitable for the determination of the enantiomer in safinamide mesilate.
6.Simultaneous Determination of 3 Optical Isomers in Carfilzomib by HPLC
Haixia LI ; Na LIU ; Peifeng BAI ; Jingyuan LIU ; Wenmin GUO
China Pharmacist 2016;19(6):1094-1095,1101
Objective:To establish an HPLC method for the determination of optical isomers in carfilzomib .Methods:The sample was separated on a Chiralpak OX-H column.The mobile phase consisted of n-hexane∶isopropanol∶alcohol (89 ∶5 ∶6, v/v/v) with a flow rat of 1.0 ml· min-1 .The detection wavelength was 220 nm.Results:The linear rang of enantiomer , diastereomer Ⅰand di-astereomer Ⅱwas 0.54-2.14 μg· ml -1,0.11-1.80 μg· ml-1 and 0.11-1.81 μg· ml-1(r≥0.998), respectively.The lower limit of quantification was 0.07-0.27 μg· ml-1 .The recoveries of optical isomers were within the range of 99.6%-100.9% with RSD of 1.13%-1.59%(n=9).Conclusion:The method is sensitive, simple, fast, accurate and specific, and suitable for the study of opti-cal isomers in carfilzomib .
7.Study on Dissolution of Ibuprofen and Paracetamol in Soft Capsules
Zhentao LIU ; Wenmin GUO ; Lifang WANG ; Li ZHANG ; Yunli LI ; Yafeng WEI
China Pharmacy 1991;0(04):-
OBJECTIVE:To determine the dissolution of ibuprofen and paracetamol in soft capsules.METHODS:Phos?phate buffer(pH=7.2)was taken as a solvent with the rotating speed set at75/min,and sample taken time was45minutes.The dissolution degree of ibuprofen and paracetamol in soft capsules were determined by a RP-HPLC method.The chro?matographic column was CN column;the mobile phase was phosphate buffer(pH=6.6)-methanol(60∶40)with a flow rate of1.0ml/min,the detection wavelength at223nm and the column temperature at30℃.RESULTS:The linear calibration curves were obtained with a range of0.17~100.14?g/ml for paracetamol(r=0.9999,n=9)and0.21~124.86?g/ml for ibuprofen(r=0.9999,n=9)respectively;the average recoveries of the two compounds were99.62%(RSD=0.36%)and99.79%(RSD=0.49%)respectively.CONCLUSION:The determination method is simple,rapid,accurate and reliable,which can be applied to measure the dissolution content of ibuprofen and paracetamol in soft capsules satisfactorily.
8.Chiral Separation and Determination of Four Lurasidone Hydrochloride Enantiomers by HPLC
Ligang ZHENG ; Xiaoxue BAI ; Wenmin GUO ; Manman WANG ; Binglin WANG ; Xuliang WANG ; Surui CHEN
China Pharmacist 2014;(2):188-190
Objective:To establish the determination method for four lurasidone hydrochloride enantiomers by HPLC. Methods:Lurasidone hydrochloride enantiomers were separated on a CHIRALPAK AD-H column (250 mm × 4. 6 mm, 5μm). The mobile phase consisted of hexane-ethanol-diethylamine ( 90∶10∶0. 1) at a flow rate of 1. 0 ml·min-1 and the column temperature was at 40℃. The detection wavelength was 230nm. Results:The resolution of lurasidone hydrochloride enantiomers was above 2. 0. The linear calibra-tion curves were obtained over the range of 5-120 μg· ml-1 for all the enantiomers (r=0. 999 9). The recovery was above 99. 0%with RSD below 0. 5%. The detection limits were 5ng. Conclusion:The method is simple, accurate and rapid, and suitable for the de-termination and quality control.
9.The effects of magnetron-sputtered ZrSiN/ZrO2 gradient coating on the bonding strength of titanium to porcelain
Xiaojing WANG ; Guowei WANG ; Guangyan HUI ; Wenmin JIA ; Yimin ZHAO ; Tianwen GUO
Journal of Practical Stomatology 2016;32(5):635-639
Objective:To evaluate the effects of magnetron-sputtered ZrSiN/ZrO2 gradient coating on the bonding strength of commercially pure titanium to porcelain.Methods:50 cast titanium specimens were prepared according to the ISO 9693 standard,and divided into 2 groups(n =25).The ZrSiN/ZrO2 gradient coating was deposited on specimens by magnetron sputtering technique,and subsequently a low-fusing porcelain was applied for the samples in the expermental group,the samples in the control group were treated by surface sandblasting.The roughness and surface energy of the samples were measured(n =10).The bonding strength of titanium-porcelain specimens was analyzed by three-point bending test (n =10).Scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDS) were employed to examine the properties of the delaminated and cross-sectioned surfaces.The results were analyzed by paired t-test (α =0.05) with SPSS 1 1.0 software.Results:The roughness of the experimantal group was lower(P < 0.05) and the contact angle was larger(P < 0.05) than those in the control group.The titanium-porcelain bond strength of gradient-coated group was greater than that of control group(P <0.05).The SEM and EDS examination results of delaminated and cross-sectioned surfaces also indicated that the gradient-coated group showed more porcelain residues.Conclusion:The bonding strength of porcelain-fused-to-titanium can be improved by magnetron sputtered ZrSiN/ZrO2 gradient coating.
10.Combining Non-Contrast CT Signs With Onset-to-Imaging Time to Predict the Evolution of Intracerebral Hemorrhage
Lei SONG ; Xiaoming QIU ; Cun ZHANG ; Hang ZHOU ; Wenmin GUO ; Yu YE ; Rujia WANG ; Hui XIONG ; Ji ZHANG ; Dongfang TANG ; Liwei ZOU ; Longsheng WANG ; Yongqiang YU ; Tingting GUO
Korean Journal of Radiology 2024;25(2):166-178
Objective:
This study aimed to determine the predictive performance of non-contrast CT (NCCT) signs for hemorrhagic growth after intracerebral hemorrhage (ICH) when stratified by onset-to-imaging time (OIT).
Materials and Methods:
1488 supratentorial ICH within 6 h of onset were consecutively recruited from six centers between January 2018 and August 2022. NCCT signs were classified according to density (hypodensities, swirl sign, black hole sign, blend sign, fluid level, and heterogeneous density) and shape (island sign, satellite sign, and irregular shape) features. Multivariable logistic regression was used to evaluate the association between NCCT signs and three types of hemorrhagic growth: hematoma expansion (HE), intraventricular hemorrhage growth (IVHG), and revised HE (RHE). The performance of the NCCT signs was evaluated using the positive predictive value (PPV) stratified by OIT.
Results:
Multivariable analysis showed that hypodensities were an independent predictor of HE (adjusted odds ratio [95% confidence interval] of 7.99 [4.87–13.40]), IVHG (3.64 [2.15–6.24]), and RHE (7.90 [4.93–12.90]). Similarly, OIT (for a 1-h increase) was an independent inverse predictor of HE (0.59 [0.52–0.66]), IVHG (0.72 [0.64–0.81]), and RHE (0.61 [0.54– 0.67]). Blend and island signs were independently associated with HE and RHE (10.60 [7.36–15.30] and 10.10 [7.10–14.60], respectively, for the blend sign and 2.75 [1.64–4.67] and 2.62 [1.60–4.30], respectively, for the island sign). Hypodensities demonstrated low PPVs of 0.41 (110/269) or lower for IVHG when stratified by OIT. When OIT was ≤ 2 h, the PPVs of hypodensities, blend sign, and island sign for RHE were 0.80 (215/269), 0.90 (142/157), and 0.83 (103/124), respectively.
Conclusion
Hypodensities, blend sign, and island sign were the best NCCT predictors of RHE when OIT was ≤ 2 h. NCCT signs may assist in earlier recognition of the risk of hemorrhagic growth and guide early intervention to prevent neurological deterioration resulting from hemorrhagic growth.