1.Progress of Chemical Derivatization in Analysis of Endogenous Anabolic Steroids in Bio-matrices
Qiuju HU ; Jianyun YANG ; Bingkun XIAO ; Rongqing HUANG
Herald of Medicine 2017;36(5):532-537
The content of endogenous anabolic steroids is extremely low in biological matrices.Its chemical structure contains polar functional groups such as hydroxyl and carbonyl, which limits their applicability in GC-MS.The lack of ionized groups in the chemical structure leads to poor sensitivity in LC-MS, which plays a significant role in various physiological activities analysis.It is an effective way to enhance the response of mass spectrometer by modifying the chemical structure of endogenous anabolic steroids through derivatization technology.This review summarizes various derivatization reagents and corresponding derivatization processes of endogenous anabolic steroids analysis in the methods based on different testing instruments and methodologies.The advantage and disadvantage of all kinds of derivatiaztion methods and the prospect of the endogenous anabolic steroids derivatiaztion techniques are also discussed.
2.Clinical results of different ways of neurotization to radial nerve
Zongyuan JIANG ; Tao WANG ; Zhujun XU ; Yudong GU ; Jianyun YANG
Chinese Journal of Trauma 2003;0(08):-
Objective To compare the result differences of different dynamic nerves transferring to different segments of the radial nerve. Methods From 1997 to 2000, different ways of intercostal nerves or contralataral C 7 transfering to different segments of the radial nerves were carried out in 36 cases with total avulsed brachial plexus injuries that were followed up for average 42.39 months. Four-fold table was selected to statistically calculate the effective rate of muscle strength recovery. Results The total effective rate was 56% (20/36). The effective rate of the functional rehabilitation of elbow extension was 5/8 in the group with neurotization to radial nerve trunk and 4/4 in the group with neurotization to branches innervating the triceps brachii muscle of radial nerve. The highest effective rate up to 75% (9/12) of the functional rehabilitation of wrist and digit extension belonged to the group with contralateral C 7 transferring to the radial nerve segment in the humeral spiral groove where branches innervating the triceps brachii muscle had already diverged. Conclusions The way of neurotization to radial nerve trunk and to branches innervating the triceps brachii muscle of the radial nerve can win good functional rehabilitation of elbow extension. Contralataral C 7 transfering to the radial nerve segment in the humeral spiral groove ranks the best way for function recovery of the wrist extension. Age below 30 years and operation interval less than 12 months are helpful for functional rehabilitation of the radial nerve.
3.A new triterpenoid fom Radix Pittospori.
Bingkun XIAO ; Weilan WANG ; Rongqing HUANG ; Jianyun YANG ; Junxing DONG
Acta Pharmaceutica Sinica 2011;46(9):1101-3
To investigate chemical constituents from Radix Pittospori, chloroform extract of the roots was subjected to column chromatography with various chromatographic techniques. The structures were elucidated on the basis of physico-chemical property and spectral analysis. Two triterpenoids were identified as 22-acetyl-21-(2-acetoxy-2-methylbutanoyl)-R1-barrigenol(1) and 3alpha-hydroxyl-20-demethylisoaleuritolic-14(15)-ene-28, 30-dioic acid (2). Compound 1 is a new triterpene and compound 2 is isolated from this plant for the first time.
4.Determination of 2-Indole Ketone Derivative and Its Related Substances by High Performance Liquid Chromatography
Yiming LI ; Bingkun XIAO ; Jianyun YANG ; Rongqing HUANG
Herald of Medicine 2016;35(4):386-389
Objective To establish an high performance liquid chromatography method for determination of 2-indole ketone derivative and its related substances. Methods Agilent Eclipse XDB-C18(250 mm×4.6 mm,5 μm) column was adopted.The mobile phase was acetonitrile-water with gradient elution mode at a flow rate of 1. 0 mL?min-1; the column temperature was 35 ℃;the injection volume was 20 μL and the detection wavelength was set at 257 nm. Results 2-indole ketone derivative ID and related substances could be well separated. The 2-indole ketone derivative had good linear correlation ( r=0.999 4) within the range of 40-300 μg?mL-1 . It had a good precision ( RSD<1%) . The limit of detection was 8 ng. Conclusion The method is accurate,simple,sensitive and selective,which can be used for the quality control of 2-indole ketone derivative and related substances.
5.Determination of content and related substances of radiosensitizer benzotriazine derivatives YABQ by HPLC
Shaolei LIU ; Jianyun YANG ; Bingkun XIAO ; Rongqing HUANG
Military Medical Sciences 2016;40(8):639-642
Objective To establish an HPLC method for determination of the content of radiosensitizer YABQ and its related substances.Methods Diamonsil C18 column (250 mm ×4.6 mm,5 μm) was used.The mobile phase consisted of methanol-0.1%formic acid (22∶78) and isocratic elution at a flow rate of 1.0 ml/min.The detection wavelength was 266 nm,the temperature of the column was 30℃, and the injection volume was 10 μl.Results The linear range of YABQ was 7-84 μg/ml, r=0.9992.The detection limit was 8 ng (S/N≥3), and the quantitation limit was 24 ng (S/N≥10). According to destructive sample processing, the separation coefficient between the peaks was above 1.5, indicating that this chromatographic method could meet the YABQ monitoring requirements.Conclusion Method validation and destructive testing show that both the precision and specificity are fine with this method, which could be used for quality control of YABQ and its related substances.
6.Determination of Contents 3-amide-indole Derivative and Related Substances
Dongni SHEN ; Jianyun YANG ; Bingkun XIAO ; Rongqing HUANG
Herald of Medicine 2014;(5):650-652
Objective To establish a RP-HPLC method for the determination of 3-amide-indole derivative and its related substances. Methods Diamonsil C18(250 mmí4. 6 mm,5 μm) column was adopted. The mobile phase consisted of a mixture of methanol-acetonitrile-water(431245) at the flow rate of 1. 0 mL·min-1 . The wavelength for ultraviolet detection was 224 nm. The injection volume was 20 μL and the column temperature was room temperature. Results 3-amide-indole derivative and related substances could be well separated. The linearity of the 3-amide-indole derivative curve was well correlated (r=0. 999 7) within the range of 0. 04-0. 16 mg·mL-1. The RSD was 0. 52%with good repeatability. The detection limit was 2. 65 ng. Conclusion The method is accurate,reliable,sensitive and specific,which could be used for the determination of 3-amide-indolederivative and related substances.
7.Effect of butorphanol and sufentanil with epidural injections on neurobehavior function in bone cancer pain model rats
Jianyun GE ; Jie SONG ; Xuefeng YANG ; Xin SUN ; Lei YAO
Chinese Journal of Behavioral Medicine and Brain Science 2016;25(6):515-519
Objective To observe the effect of different doses of butorphanol and sufentanil repeatedly epidural injected on the neurobehavior function in bone cancer model rats.Methods A PE-530 catheter was inserted into the epidural space of all male Sprague-Dawley rats(not mated,weighting 150-180 g) at L1-2 level.Three days after operation,64 rats without any motor dysfunction were randomly divided into eight groups (n=8):sham operated group (group C),normal saline with bone cancer pain group (group N),butorphanol groups(group B 1,B2,B3)and sufentanil groups (group S1,S2,S3).Bone cancer pain model was constructed in group N,B and S when rats in group C were sham operated.Rats in group C and N were epidurally injected NS 30μl each,and rats in group B1,B2 and B3 were respectively epidurally injected butorphanol 25,50,100 μg (all diluted to 30 μl with NS),when rats in group S1,S2 and S3 were respectively cpidurally injected sufentanil 1,2,4 μg (all diluted to 30 μl with NS) on time per day for 10-14 days after modeling.The neurobehavior paw withdrawal threshold (MWT) of the left hind claw was recorded to observe the changes in pain behavior.The neurobehavior function of rats were recorded by BBB (BASSO,BEATTIE and BRESNAHAN) score and the inclined plane test.Results Compared with group C((67.65±9.29) g),the MWT of the model groups obviously decreased before the first time of injection (N (15.23± 2.46) g,B 1 (16.14±2.28) g,B2(15.42±3.22) g,B3(14.35±2.32) g,S1 (15.37±2.11)g,S2(15.22±2.93) g,S3(16.25± 2.36) g) (all P<0.05)).Compared with group N((16.13±2.37) g),the MWT of group B2,B3 and S3 increased obviously after the first time of injection ((35.12±5.16) g,(35.63± 1.53) g and (34.24±5.93) g) (P< 0.05).At the first day of injection,there was no significant difference in the BBB scores and the inclined plane test between the model groups (P>0.05).At 6 h after the forth injection the inclined plane test and the BBB scores of group B3 were obviously decreased compared with group N ((34.72 ± 4.56) ° and (10.64 ± 1.82) points to (43.15±4.67)° and (14.05±1.78) points (P<0.05)).Conclusion The results provide evidence that repeatedly epidural injection of butorphanol 50 μg or 100 μg or sufentanil 4 μg can reduce the pain of the rats with bone cancer pain.But repeated epidural injection of butorphanol 100 μg can injure the neurological function.
8.THE DYNAMIC CHANGES OF PLASMA AND ERYTHROCYTE RIBOFLAVIN AND ITS DERIVATIVES CONCENTRATIONS IN RIBOFLAVIN DEFICIENT RATS
Qishou XU ; Jingyu WEI ; Jijun YANG ; Jianyun YANG ; Yonghui LI ; Jing XU
Acta Nutrimenta Sinica 2004;0(05):-
Objective: To investigate the dynamic changes of plasma and erythrocyte riboflavin and its derivatives concentrations after riboflavin deficiency and so as to provide theoretic basis for their application in riboflavin status assessment. Methods: The riboflavin deficiency was induced in rats by feeding a riboflavin deficient diet. The plasma and erythrocyte riboflavin and its derivatives (FMN and FAD) were analysed with HPLC method. The blood glutathione reductase activity coefficient (BGRAC), erythrocyte GSH concentration and urinary riboflavin excretion were also measured. Results: The plasma riboflavin concentration as well as the urinary riboflavin excretion were decreased rapidly early after riboflavin deficiency and followed by plasma riboflavin derivatives. The erythrocyte riboflavin and its derivatives and GSH concentrations were decreased significantly later. On the other hand, the BGRAC was increased significantly in the early period of riboflavin deficiency and the change, however, was limited in a narrow range. Conclusion: The plasma and erythrocyte riboflavin concentration can be applied as a marker in riboflavin status assessment but human studies are necessary for further research.
9.A study on reference memory and working memory of pure cerebral concussion and multiple cerebral concussion by 8-arm radial maze in rats
Zhenzhen CAO ; Jianyun YU ; Qiao ZHU ; Zeyun GUO ; Li YANG ; Huan ZHANG ; Yanyu QU
Chinese Journal of Behavioral Medicine and Brain Science 2010;19(4):296-299
Objective To observe learning and memory behavior changes of one time cerebral concussion called pure cerebral concussion(PCC)and three times cerebral concussion called multiple cerebral concussion (MCC)after injured 24 days in rats.Methods A metallic pendulum striker device was deployed to duplicate PCC and MCC model in SD rata which were the complete closed head injury model.The animals were divided into PCC and MCC groups at random.One control group was used,each group has eight animals(n=8).One 8-arms radial maze was used to assessed each animal's capabilities,that is,spatial reference memory,working memory,spirited activity and take in food.Results Compared with control group,there were some significance(P<0.05)in both experiment groups post injury,that was,(1)The food intake decreased,PCC group from the 1st to the 11th day(from 0.00±0.00 to 2.62±1.76)after injury,MCC group from the 1st day to the 24th day(from 0.00±0.00 to 0.75±1.48)after injury.(2)Spirited activity depressed,PCC group on the 1st to the 7th,13rd day(from 4.87±1.24 to 10.0±2.39)after injury,MCC group on the 1st to 8th,22nd day(from 4.25±5.03 to 9.37±4.20)after injury.(3)The spatial reference memory was lower in early then gradually increased,PCC group on the 1 st to 7th day(from 0.50±0.75 to 3.O0±1.06)after injury,MCC group from the 1st to 19th day(from 1.88±2.10 to 2.50±2.44)after injury.(4)The working memory was delaying damaged,PCC group from the 1st to the 6th day and the 10th to the 23rd day(from 0.00±0.00 to 4.25±3.05)after injury,MCC group on the 1~4th,6th,9~13th,15th,16th,19th~22nd day(from 0.25±0.46 to 3.12±2.87)after injury.Conclusion The injured rata'capability of spatial reference memory,working memory,spirited activity and food intake were obviously damaged after CC,and the MCC group's capability of spatial reference memory,spirited activity and food intake was worse than PCC group.
10.Powder modification technology used for the preparation of the hydrophilic decoction pieces of indigo naturalis and the modification principle.
Dingkun ZHANG ; Junzhi LIN ; Jianyun LIU ; Chunfeng QIN ; Zhiping GUO ; Li HAN ; Ming YANG
Acta Pharmaceutica Sinica 2013;48(7):1148-55
The hydrophilicity of the normal decoction pieces (NDP) of Indigo Naturalis is not good, therefore, it is not suit for decoctions. In this paper, powder modification technology is used and some NDP and alcohol are ground together in the vibromill to prepare the hydrophilic decoction pieces (HDP) of Indigo Naturalis. Initially, the properties of NDP, ultrafine decoction pieces (UDP) and HDP are compared, the hydrophilicity of UDP was promoted slightly, that of HDP is promoted dramatically. Then, three batches of Indigo Naturalis are prepared to HDP separately, but there is no obvious difference in the contact angle. Furthermore, the size distribution, surface area and micro-shape of HDP are bigger than that of UDP and smaller than NDP. The contents of indigo and indirubin in three decoction pieces are the same, as well as the species of inorganic substance, although there is a little difference in the proportion of five inorganic substances. The fact suggests the change of physical state and the qualitative and quantitative change of organism and inorganic substances are not the main factors to influence the hydrophilicity. In addition, hydroxyl, methylene and methyl can be identified at the wavenumber of 3 356 cm(-1) and 1 461 cm(-1) in infrared spectrum; the content of alcohol in HDP is 0.67% measured by gas chromatogram. The stability of HDP in the heating condition is studied, the fact suggests the hydrophilic effect of HDP at 40 degrees C is relatively stable. All above research suggests that the alcohol is the main factor to influence the hydrophilicity and maybe the intermolecular force which fixed alcohol molecule on the surface of Indigo Naturalis is the basic principle to produce the hydrophilicity.