Objective:To establish a high-performance liquid chromatography(HPLC)method for the determina-tion of related substances in buprenorphine active pharmaceutical ingredient(API)using advanced ACD/Auto-Chrom method development software for comprehensive parameter simulation and design.Methods:An Agilent ZORBAX Eclipse Plus C18 column(4.6 mm × 150 mm,3.5 μm)was used with a mobile phase consisting of 40 mmol·L-1 potassium dihydrogen phosphate solution and acetonitrile in a gradient elution mode.The flow rate was set at 1.3 mL·min-1,the column temperature was maintained at 35 ℃,the detection wavelength was 240 nm,and the injection volume was 5 μL.Results:The impurities A,B,D,E,F,G,H,I,and J in buprenorphine were effectively separated from the main component.The linear ranges were 0.33-83.73,0.20-78.74,0.20-40.28,0.22-43.31,0.32-78.98,0.13-63.74,0.51-101.54,0.22-43.72,and 0.40-80.37 μg·mL-1,respectively.The limits of detection(LOD)were 0.10,0.06,0.06,0.06,0.09,0.04,0.15,0.07,and 0.12 μg·mL-1,respectively,while the limits of quantification(LOQ)were 0.33,0.20,0.20,0.22,0.32,0.13,0.51,0.22,and 0.40 μg·mL-1,respectively.The accuracy,precision,and robustness of the method met the required standards.Conclusion:This method is suitable for the determi-nation and quality control of related substances such as impurities A,B,D,E,F,G,H,I,and J in buprenorphine API.

Objective:With the help of the advanced ACD Labs/AutoChrom method development software,param-eter simulation design was carried out.Based on the results of software simulation and actual investigation,an HPLC method for the determination of related impurities in safinamide mesylate raw material drug was established.Methods:A Waters Atlantis T3 column(4.6 mm ×250 mm,5 μm)was used.The phosphate buffer with a pH of 7.0 was used as mobile phase A,and acetonitrile was used as mobile phase B.Gradient elution was performed at a flow rate of 1.3 mL·min-1,the detection wavelength was 228 nm,the column temperature was 35 ℃,and the injection volume was 10 μL.Results:Impurities 1-12 in safinamide mesylate could be effectively separated from the main component.The linear ranges were 0.102 1-5.329,0.102 9-5.379 7,0.106 8-4.972 9,0.102 1-5.135,0.103 8-5.314 7,0.097 7-4.869 8,0.095 2-4.760 5,0.095 3-5.109 5,0.050 5-5.287 5,0.098 7-4.885 6,0.102 4-4.997 5,0.050 8-5.134 7 μg·mL-1,respectively.The limits of detection(LOD)were 0.051,0.051 4,0.053 4,0.051 1,0.051 9,0.048 8,0.047 6,0.047 7,0.025 3,0.049 3,0.051 2,0.025 4 μg·mL-1,and the limits of quantification(LOQ)were 0.102 1,0.102 9,0.106 8,0.102 1,0.103 8,0.097 7,0.095 2,0.095 3,0.050 5,0.098 7,0.102 4,0.050 8 μg·mL-1.The accuracy,preci-sion and durability all met the requirements.Conclusion:This method is suitable for the determination and quality control of the related substances of 12 impurities in safinamide mesylate raw materials.

Objective:With the help of the advanced ACD Labs/AutoChrom method development software,param-eter simulation design was carried out.Based on the results of software simulation and actual investigation,an HPLC method for the determination of related impurities in safinamide mesylate raw material drug was established.Methods:A Waters Atlantis T3 column(4.6 mm ×250 mm,5 μm)was used.The phosphate buffer with a pH of 7.0 was used as mobile phase A,and acetonitrile was used as mobile phase B.Gradient elution was performed at a flow rate of 1.3 mL·min-1,the detection wavelength was 228 nm,the column temperature was 35 ℃,and the injection volume was 10 μL.Results:Impurities 1-12 in safinamide mesylate could be effectively separated from the main component.The linear ranges were 0.102 1-5.329,0.102 9-5.379 7,0.106 8-4.972 9,0.102 1-5.135,0.103 8-5.314 7,0.097 7-4.869 8,0.095 2-4.760 5,0.095 3-5.109 5,0.050 5-5.287 5,0.098 7-4.885 6,0.102 4-4.997 5,0.050 8-5.134 7 μg·mL-1,respectively.The limits of detection(LOD)were 0.051,0.051 4,0.053 4,0.051 1,0.051 9,0.048 8,0.047 6,0.047 7,0.025 3,0.049 3,0.051 2,0.025 4 μg·mL-1,and the limits of quantification(LOQ)were 0.102 1,0.102 9,0.106 8,0.102 1,0.103 8,0.097 7,0.095 2,0.095 3,0.050 5,0.098 7,0.102 4,0.050 8 μg·mL-1.The accuracy,preci-sion and durability all met the requirements.Conclusion:This method is suitable for the determination and quality control of the related substances of 12 impurities in safinamide mesylate raw materials.

Objective:To establish a high-performance liquid chromatography(HPLC)method for the determina-tion of related substances in buprenorphine active pharmaceutical ingredient(API)using advanced ACD/Auto-Chrom method development software for comprehensive parameter simulation and design.Methods:An Agilent ZORBAX Eclipse Plus C18 column(4.6 mm × 150 mm,3.5 μm)was used with a mobile phase consisting of 40 mmol·L-1 potassium dihydrogen phosphate solution and acetonitrile in a gradient elution mode.The flow rate was set at 1.3 mL·min-1,the column temperature was maintained at 35 ℃,the detection wavelength was 240 nm,and the injection volume was 5 μL.Results:The impurities A,B,D,E,F,G,H,I,and J in buprenorphine were effectively separated from the main component.The linear ranges were 0.33-83.73,0.20-78.74,0.20-40.28,0.22-43.31,0.32-78.98,0.13-63.74,0.51-101.54,0.22-43.72,and 0.40-80.37 μg·mL-1,respectively.The limits of detection(LOD)were 0.10,0.06,0.06,0.06,0.09,0.04,0.15,0.07,and 0.12 μg·mL-1,respectively,while the limits of quantification(LOQ)were 0.33,0.20,0.20,0.22,0.32,0.13,0.51,0.22,and 0.40 μg·mL-1,respectively.The accuracy,precision,and robustness of the method met the required standards.Conclusion:This method is suitable for the determi-nation and quality control of related substances such as impurities A,B,D,E,F,G,H,I,and J in buprenorphine API.

This study reviewed 37 patients who received neoadjuvant ADT in our center and analyzed the change of 68Ga-PSMA PET/CT before and after treatment. This study found that neoadjuvant ADT significantly reduced the tumor visibility on 68Ga-PSMA PET/CT.

Objective To investigate the clinical values of the leukocyte count,D-dimer,histidine decarboxylase (HDC) and intestinal fatty acid binding protein (I-FABP) for diagnosing acute intestinal obstruction.Methods Sixty patients who treated in China-Japan Union Hospital of Jilin University from January 2017 to January 2018 were collected prospectively,and were divided into strangulated intestinal obstruction (STR-IO) group (n =20),simple intestinal obstruction (SIM-IO) group (n =20) and peritonitis group (n =20).Twenty healthy volunteers were collected as control group.Automatic blood cell analyzer was used to detecting the leukocyte count.The concentration of plasma D-dimer was detected by immune turbidimetry method.The concentration of serum HDC and I-FABP were measured by enzyme linked immunosorbent assay (ELISA) method.Compared the above indicators of four groups of samples.The measurement data are expressed as mean ± standard deviation (Mean ± SD).Tamhane's T2 and Dunnett's T3 methods were used to comparison between groups.Estimation of receiver operating characteristic curve(ROC) and area under curve (AUC) used logistic regressive model.Results The leukocyte count in control group,SIM-IO group,peritonitis group,and STR-IO group were (6.97 ± 1.68) × 109/L,(8.24 ± 2.78) × 109/L,(11.33 ±4.75) × 109/L,and(12.53 ± 5.96) × 109/L respectively.STR-IO group and peritonitis group were significantly higher than those of control group(F =12.74,P =0.01),but there was no significant difference between SIM-IO group and control group(P ＞ 0.05).The concentration of plasma D-dimer in control group,SIM-IO group,peritonitis group,and STR-IO group were (0.44± 0.30) μg/ml,(1.17 ± 0.67) μg/ml,(1.20 ± 0.72) μg/ml,and (1.67 ± 0.67) μg/ml respectively.The concentration of D-dimer in STR-IO group was significantly higher than those of control group (F =57.08,P =0.00),and there was no significant difference among other group (P ＞ 0.05).The concentration of serum HDC in control group,SIM-IO group,peritonitis group,and STR-IO group were (5.51 ±4.30) ng/ml,(14.33 ± 3.71) ng/ml,(11.53 ± 4.67) ng/ml,and (35.65 ± 21.15) ng/ml respectively.The concentration of HDC in STR-IO group was significantly higher than those of other three groups (F =39.03,P =0.00).The concentration of serum I-FABP in control group,SIM-IO group,peritonitis group,and STR-IO group were (0.20 ± 0.06) ng/m],(0.31 ± 0.17) ng/ml,(0.22 ±0.03)ng/ml,and (0.81 ±0.56) ng/ml respectively.The concentration of I-FABP in STR-IO group was significantly higher than those of other three groups (F =23.07,P =0.01).The AUC of HDC,I-FABP,D-dimer,and leukocyte count were 0.998,0.868,0.730,and 0.704 respactively.Conclusion Leukocyte count,D-dimer,and HDC or I-FABP combined detection may be a more effective index for diagnosing acute intestinal obstruction.

Objective To analyze crossed cerebellar diaschisis(CCD) after subacute phase of spontaneous cerebral hemorrhage(SPSCH)and it's relevant factors with whole-brain CT perfusion(CTP) imaging. Methods Eighty-six patients diagnosed with unilateral SPSCH by CT were prospectively enrolled in our study from July 2015 to October 2016. Whole-brain CTP was performed in each patient.Cerebral blood flow(CBF), cerebral blood volume(CBV), mean transit time(MTT)and time-to-peak(TTP) inipsilateral and contralateral cerebellum were manually measured.The asymmetric indexs(AIs) were also calculated. Moreover, the volume of hematoma, the maximumarea of peri-hematomahypoperfusionin CBF and clinical factors(age, gender, time intervals from symptom onset)were analyzed,and NIHSS scores were used to evaluate the neurological status before patient admission, inspection, and discharge.CCD was rated positive when a unilateral supratentorial hematomawas appeared and an accompanying perfusion decrease was showed in the contralateral cerebellum on at least two sequential slices of CTP maps.All the individuals were divided into two groups including CCD-positive groupand CCD-negative group. The perfusion parameters (CBF, CBV, MTT, and TTP)between the contralateral and ipsilateral cerebellum were analyzed by the two-tailed paired t-test in CCD-positive group. The differences in the perfusion and clinical variables between the two groups were analyzed by the independent sample t-test and the Chi-squared test. Therelationships between the AI values and clinical or radiologic variables were assessed with Pearson correlation test. Results We found 35 CCD positive cases and 51 negative cases in the 86 patients.In CCD-positive groups, the perfusion values of cerebellumipsilateral and contralateral to the hematomawere as follows:CBF were (40.88±11.23) vs. (33.91±9.96) ml·100 g-1·min-1, CBV were (3.30±1.18) vs. (2.75±1.13) ml/100 g and TTP were (22.09±3.98) vs. (22.88±4.15) s, respectively, and there was statistical significance (t=10.231,8.223,-2.883,P<0.05).In CCD positive group, CBF, CBV, TTP, and MTT of the contralateral cerebellar hemisphere was changed in 35, 32, 26, and 16 cases,respectively.The AI value of CBF(AICBF)in CCD-positive group was (17.10±9.10)%, which was higher than that in the negative group (-0.95±17.01)%, there was statistical significance(t=6.367,P<0.05).The AI value of CBV(AICBV)was (17.43 ± 11.65)% in CCD-positive group, also significantly higher than that in negative group which was (1.55±21.06)%(t=4.477, P<0.05). No statistical difference(P>0.05)was found in hematoma location,hematoma volume, supratentorialhypoperfusion area and NIHSS scores(at admission, inspection)between CCD-positive and negative groups.The AICBF and AITTP showed linear correlation with time intervals in CCD-positive patients(P<0.05). Conclusions CCD is a common phenomenon in patients with SPSCH.Of all the perfusion parameters,CBF abnormalities are more common.The severity of CCD has a certain correlation with time intervals.There is no significant correlation between CCD and the clinical or radiological data(age, NIHSS scores,hematoma volume, and supratentorial hypoperfusion area).

The inflammatory reaction of renal tissues and its relevant tissue damages (such as glomerulosclerosis and renal interstitial fibrosis) are important factors for the development of chronic kidney diseases (CKD) to end-state renal diseases. Of them, p38 mitogen-activated protein kinase (MAPK) signaling pathway plays an important role in regulating expression and bioactivity of multiple nuclear transcription factors, impacting synthesis of downstream inflammatory mediators and activating inflammatory cells. Some monomer traditional Chinese medicines and their extracts (such as emodin and berberine) and some traditional Chinese medicine compound prescriptions (such as Yishen Huoxue decoction) can affect inflammatory reaction of renal tissues by regulating p38MAPK signaling pathway, thas improving reduce glomerulus and renal interstitial inflammatory injury.
Animals ; Chronic Disease ; Humans ; Inflammation ; drug therapy ; pathology ; Kidney Diseases ; drug therapy ; pathology ; Medicine, Chinese Traditional ; methods ; Signal Transduction ; drug effects ; p38 Mitogen-Activated Protein Kinases ; metabolism