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1.
PhytoKeys ; 211: 63-73, 2022.
Article in English | MEDLINE | ID: mdl-36760724

ABSTRACT

A new species of Gesneriaceae from Guizhou, China, Hemiboeakaiyangensis sp. nov., is described and illustrated. We investigated its phylogenetic position and relationships with 13 other species of Hemiboea C.B.Clarke, which present large morphological diversity in the genus, based on molecular analyses of the nuclear ribosomal internal transcribed spacer (ITS) and the chloroplast trnL-F intron-spacer sequences. The molecular phylogenetic analyses revealed that the new species is most closely related to H.ovalifolia. A diagnostic table and discussion of morphological characters are provided to differentiate the new species from H.longisepala, H.flaccida and H.ovalifolia.

2.
J Plant Physiol ; 224-225: 56-67, 2018.
Article in English | MEDLINE | ID: mdl-29597068

ABSTRACT

Seed germination is a critical process that is influenced by various factors. In the present study, the effect of low temperature (4 °C) on tree peony seed germination was investigated. Compared to seeds maintained at 25 °C, germination was inhibited when seeds were kept at 4 °C. Furthermore, low-temperature exposure of seeds resulted in a delay in water uptake, starch degradation, and soluble sugar consumption and a subsequent increase in soluble protein levels. Two-dimensional gel electrophoresis (2-DE) proteomic analysis identified 100 protein spots. Comparative analysis indicated that low-temperature exposure apparently mainly affected glycolysis and the tricarboxylic acid (TCA) cycle, while also significantly affecting proteometabolism-related factors. Moreover, low-temperature exposure led to the induction of abscisic acid, whereas the gibberellin pathway was not affected. Further comparison of the two temperature conditions showed that low-temperature exposure delays carbohydrate metabolism, adenosine triphosphate (ATP) production, respiration, and proteolysis and increases defense response factors. To further examine the obtained proteomic findings, four genes were evaluated by quantitative polymerase chain reaction (qPCR). The obtained transcriptional results for the GAPC gene coincided with the translational results, thus further suggesting that the delay in glycolysis may play a key role in low-temperature-induced inhibition of seed germination. However, the other three genes examined, which included FPP synthase, PCNT115, and endochitinase, showed non-correlative transcriptional and translational profiles. Our results suggest that the exposure of tree peony seeds to low temperature results in a delay in the degradation of starch and other metabolites, which in turn affects glycolysis and some other processes, thereby ultimately inhibiting seed germination.


Subject(s)
Germination , Paeonia/genetics , Plant Proteins/genetics , Proteome , Transcriptome , Cold Temperature , Germination/genetics , Paeonia/growth & development , Plant Proteins/metabolism , Seeds/genetics , Seeds/growth & development
3.
Acta Trop ; 153: 101-10, 2016 Jan.
Article in English | MEDLINE | ID: mdl-26482137

ABSTRACT

Leishmania spp. are able to survive and proliferate inside mammals' mononuclear phagocytes, causing Leishmaniasis. Previous studies have noted that the regulation of apoptosis in host cells by these parasites may contribute to their ability to evade the immune system. However, current results remain unclear about whether the parasites can promote or delay the apoptotic process in host cells, because the regulatory effect of Leishmania was assumed to be strain-, species- and even infection time-dependent. The aim of this study was to investigate whether the Sichuan isolates of Chinese Leishmania (SC10H2) can alter the process of intrinsic apoptosis induced by cycloheximide in different types of macrophage cell lines and to determine in which steps of the signaling pathway the parasites were involved. Human THP-1 and mouse RAW264.7 macrophages were infected by SC10H2 promastigotes followed by cycloheximide stimulation to assess the alteration of intrinsic apoptosis in these cells. The results indicated that SC10H2 infection of human THP-1 macrophages could promote the initiation of intrinsic apoptosis, but completely opposite results were found in mouse RAW264.7 macrophages. Nevertheless, the expression of Bcl-2 and the DNA fragmentation rates were not altered by SC10H2 infection in the cell lines used in the experiments. This study suggests that SC10H2 promastigote infection is able to promote and delay the transduction of early apoptotic signals induced by cycloheximide in THP-1 and RAW264.7 macrophages, revealing that the regulation of intrinsic apoptosis in host cells by SC10H2 in vitro occurs in a host cell-dependent manner. The data from this study might play a significant role in further understanding the relationship between Leishmania and different host cells.


Subject(s)
Antiprotozoal Agents/therapeutic use , Apoptosis/drug effects , Cycloheximide/therapeutic use , Leishmaniasis/drug therapy , Leishmaniasis/immunology , Macrophages/drug effects , Macrophages/parasitology , Animals , Cell Line/drug effects , Humans , Leishmania/drug effects , Mice
4.
Guang Pu Xue Yu Guang Pu Fen Xi ; 34(12): 3288-91, 2014 Dec.
Article in Chinese | MEDLINE | ID: mdl-25881425

ABSTRACT

By analyzing HyJet V phosphate ester hydraulic oil environmental impacts (oil, etc.) and confounding factors (pH, temperature, etc.), the feasibility was studied for the fluorescence detection of aircraft hydraulic oil leaks. By using the fluorescence spectrophotometer at various acidities and temperatures, the fluorescence properties of HyJet V phosphate ester hydraulic oil, Jet Oil II lubricant and 2197 lubricant were gained. The experimental results are shown as following: The fluorescence peaks of HyJet V phosphate ester hydraulic oil, Jet Oil II lubricant and 2197 lubricant are at 362, 405 and 456 nm, respectively. The impact of temperature on HyJet V phosphate ester hydraulic oil is less effective; Jet Oil II lubricant and 2197 lubricant fluorescence intensity decreases with increasing temperature. When acidity increases, the fluorescence peak of HyJet V phosphate ester hydraulic oil gradient shifts from 370 to 362 nm, and the fluorescence intensity decreases; the fluorescence peak of Jet Oil II lubricant is always 405 nm, while the fluorescence intensity decreases; the fluorescence peak of 2197 lubricant at 456 nm red shifts to 523 nm, and double fluorescence peaks appeare. The results are shown as following: under the influence of the environment and interference factors, the fluorescence characteristics of HyJet V phosphate ester hydraulic oil remain unchanged, and distinguish from Jet Oil II lubricant and 2197 lubricant. Therefore, the experiments indicate that the detection of HyJet V phosphate ester hydraulic oil leak is feasible by using fluorescence method.

5.
Zhongguo Ying Yong Sheng Li Xue Za Zhi ; 29(5): 457-60, 2013 Sep.
Article in Chinese | MEDLINE | ID: mdl-24386828

ABSTRACT

OBJECTIVE: To illustrate the molecular mechanism of skeletal muscle growth by examining the effect of swimming training on skeletal muscle growth and p70s6k, rpS6 protein expression. METHODS: Twenty four male SD rats were used to establish swimming training models with a 15% body mass load. The training protocol adopted interval swimming training (every other day with 8 weeks). The gastrocnemius and soleus muscle were collected and weighed after training, and the protein expression of p70s6k, rpS6 and their phosphorylated forms were examined. RESULTS: After 8 weeks treatment, no significant change was observed in skeletal muscle mass between training group (T) and control group (C) (P > 0.05), but muscle mass in training rapamycin (TR) group has a significantly decrease compared with that in T and C groups (P < 0.05). Soleus and gastrocnemius muscle mass index in T group increased significantly compared with C group (P < 0.05). Compared with the C group, the ratio of P-p70s6k/p70s6k in T group increased with significant difference (P < 0.05), but the ratio in TR group was significantly reduced (P < 0.05). The ratio of P-rpS6/rpS6 had a significant difference between TR and T group (P < 0.05). CONCLUSION: These results suggest that the interval training protocol is helpful to increase the relative muscle hypertrophy, and has a role in promoting the expression of p70s6k and rpS6.


Subject(s)
Muscle, Skeletal/metabolism , Physical Conditioning, Animal , Ribosomal Protein S6 Kinases, 70-kDa/metabolism , Swimming , Animals , Male , Muscle, Skeletal/growth & development , Muscle, Skeletal/physiology , Rats , Rats, Sprague-Dawley
6.
Adv Drug Deliv Rev ; 64(5): 461-78, 2012 Apr.
Article in English | MEDLINE | ID: mdl-22300653

ABSTRACT

The solid-state chemistry of drugs has seen growing importance in the pharmaceutical industry for the development of useful API (active pharmaceutical ingredients) of drugs and stable dosage forms. The stability of drugs in various solid dosage forms is an important issue because solid dosage forms are the most common pharmaceutical formulation in clinical use. In solid-state stability studies of drugs, an ideal accelerated method must not only be selected by different complicated methods, but must also detect the formation of degraded product. In this review article, an analytical technique combining differential scanning calorimetry and Fourier-transform infrared (DSC-FTIR) microspectroscopy simulates the accelerated stability test, and simultaneously detects the decomposed products in real time. The pharmaceutical dipeptides aspartame hemihydrate, lisinopril dihydrate, and enalapril maleate either with or without Eudragit E were used as testing examples. This one-step simultaneous DSC-FTIR technique for real-time detection of diketopiperazine (DKP) directly evidenced the dehydration process and DKP formation as an impurity common in pharmaceutical dipeptides. DKP formation in various dipeptides determined by different analytical methods had been collected and compiled. Although many analytical methods have been applied, the combined DSC-FTIR technique is an easy and fast analytical method which not only can simulate the accelerated drug stability testing but also at the same time enable to explore phase transformation as well as degradation due to thermal-related reactions. This technique offers quick and proper interpretations.


Subject(s)
Diketopiperazines/chemistry , Dipeptides/chemistry , Calorimetry, Differential Scanning , Drug Stability , Spectroscopy, Fourier Transform Infrared
7.
Int J Mol Sci ; 13(12): 16065-83, 2012 Nov 29.
Article in English | MEDLINE | ID: mdl-23443111

ABSTRACT

A comparative proteomic analysis of drought-responsive proteins during grain development of two wheat varieties Kauz (strong resistance to drought stress) and Janz (sensitive to drought stress) was performed by using linear and nonlinear 2-DE and MALDI-TOF mass spectrometry technologies. Results revealed that the nonlinear 2-DE had much higher resolution than the linear 2-DE. A total of 153 differentially expressed protein spots were detected by both 2-DE maps, of which 122 protein spots were identified by MALDI-TOF and MALDI-TOF/TOF mass spectrometry. The identified differential proteins were mainly involved in carbohydrate metabolism (26%), detoxification and defense (23%), and storage proteins (17%). Some key proteins demonstrated significantly different expression patterns between the two varieties. In particular, catalase isozyme 1, WD40 repeat protein, LEA and alpha-amylase inhibitors displayed an upregulated expression pattern in Kauz, whereas they were downregulated or unchanged in Janz. Small and large subunit ADP glucose pyrophosphorylase, ascorbate peroxidase and G beta-like protein were all downregulated under drought stress in Janz, but had no expression changes in Kauz. Sucrose synthase and triticin precursor showed an upregulated expression pattern under water deficits in both varieties, but their upregulation levels were much higher in Kauz than in Janz. These differentially expressed proteins could be related to the biochemical pathways for stronger drought resistance of Kauz.


Subject(s)
Gene Expression Regulation, Plant , Plant Proteins/biosynthesis , Proteome/biosynthesis , Triticum/metabolism , Dehydration/genetics , Dehydration/metabolism , Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization
8.
Analyst ; 136(5): 1036-40, 2011 Mar 07.
Article in English | MEDLINE | ID: mdl-21183974

ABSTRACT

The combination of Fourier transform infrared (FT-IR) microspectroscopy with a thermal analyzer was applied to quickly investigate the solid-state ion-exchange reaction of metoclopramide HCl monohydrate (MCP H(2)O) by clipping MCP H(2)O powder between two KBr or KCl pellets. The physical and ground mixtures of MCP H(2)O or 150 °C-preheated MCP powder and KBr or KCl powders with a weight ratio of 1 : 100 were also prepared and determined by FT-IR microspectroscopy. The samples of MCP H(2)O or 150 °C-preheated MCP were identified by using differential scanning calorimetry (DSC) and thermogravimetric (TG) analysis. The results of present study indicate that the ion-exchange reaction was easily induced between MCP H(2)O and KBr by grinding and heating processes. The possible mechanism of ion-exchange reaction may take place between the HCl salt of MCP H(2)O and a KBr matrix by grinding or heating to yield a mixture of HCl and HBr salts of the MCP sample in the presence of hydrated water. The crystal hydrate played an important role to improve this ion-exchange reaction between MCP H(2)O and KBr. However, no ion-exchange reaction occurred between MCP H(2)O and KCl or between 150 °C-preheated MCP and KBr. The solid-state ion-exchange reaction was more easily determined by this novel thermal FT-IR microspectroscopy than other conventional methods.


Subject(s)
Bromides/analysis , Ion Exchange , Metoclopramide/analysis , Potassium Compounds/analysis , Spectroscopy, Fourier Transform Infrared/methods , Calorimetry, Differential Scanning/methods , Hot Temperature
9.
Ultrason Imaging ; 32(1): 1-15, 2010 Jan.
Article in English | MEDLINE | ID: mdl-20690428

ABSTRACT

Speckle tracking has been used for motion estimation in ultrasound imaging. Unlike conventional Doppler techniques, which are angle-dependent, speckle tracking can be utilized to estimate velocity vectors. However, the accuracy of speckle-tracking methods is limited by speckle decorrelation, which is related to the displacement between two consecutive images, and, hence, combining high-frame-rate imaging and speckle tracking could potentially increase the accuracy of motion estimation. However, the lack of transmit focusing may also affect the tracking results and the high computational requirement may be problematic. This study therefore assessed the performance of high-frame-rate speckle tracking and compared it with conventional focusing. The effects of the signal-to-noise ratio (SNR), bulk motion, and velocity gradients were investigated in both experiments and simulations. The results show that high-frame-rate speckle tracking can achieve high accuracy if the SNR is sufficiently high. In addition, its computational complexity is acceptable because smaller search windows can be used due to the displacements between frames generally being smaller during high-frame-rate imaging. Speckle decor-relation resulting from velocity gradients within a sample volume is also not as significant during high-frame-rate imaging.


Subject(s)
Hemorheology , Ultrasonography, Doppler/methods , Image Processing, Computer-Assisted , Motion , Phantoms, Imaging , Signal Processing, Computer-Assisted
10.
Article in English | MEDLINE | ID: mdl-19942498

ABSTRACT

Some success has been demonstrated in the extensive studies of adaptive imaging, but these approaches are generally not suitable for high-frame-rate (HFR) imaging where broad transmit beams are required. In this study, we propose an effective adaptive imaging method suitable for HFR imaging based on coherence-factor (CF) weighting and the minimum-variance-distortionless-response (MVDR) method. The CF is an index of focusing quality estimated from receive-channel data in which the amplitude of each image pixel is weighted by the corresponding CF so as to reduce the unwanted sidelobes. Direct implementation of CF weighting in HFR imaging does not provide satisfactory results because the broad transmit beams required for HFR imaging reduce the accuracy of CF calculations. In this study, we alleviated this problem by applying the MVDR method. We test the proposed method with the synthetic transmit aperture method where only 8 firings are required to form an image. Both simulations and clinical breast imaging data were used, and the proposed method enhanced the mean contrast by around 4.6 dB and the mean contrast-to-noise ratio by around 20%. The results demonstrate that the proposed method is effective at improving the image quality.


Subject(s)
Signal Processing, Computer-Assisted , Ultrasonography, Mammary/methods , Adult , Aged , Algorithms , Breast , Breast Neoplasms/diagnostic imaging , Computer Simulation , Humans , Middle Aged , Phantoms, Imaging , Transducers
11.
Drug Dev Ind Pharm ; 34(12): 1368-75, 2008 Dec.
Article in English | MEDLINE | ID: mdl-18720143

ABSTRACT

Differential scanning calorimetry (DSC) combined with a curve-fitting program was utilized to quantitatively determine the polymorphic composition of famotidine in the compacts prepared by different compression treatments. Two types of famotidine compacts (compact I or II) were prepared by compressing a conical shape or a flattened shape of powder bed of famotidine form B. The compact I was constructed by a transparent region in the center with an opaque region surrounded outside, but the compact II was formed by a whole opaque region only. A drilled disc sample was prepared and then directly determined by DSC analysis. The Raman spectral results clearly indicate that all the compacts whether in any region before DSC determination were only of famotidine form B and independent of compression pressure applied. Under DSC determination, however, the curve-fitted relative compositions of form B in the drilled disc I sample were gradually reduced to 23-24% with the increase of compression pressure, whereas the curve-fitted relative composition of form A was slowly increased up to 76-77%. A transitional phase of famotidine form B (form B*) in the transparent region of the compact I after applying >150 kg/cm(2) of compression pressure was easily detected, and then transformed to famotidine form A under DSC heating process. But this transitional phase and polymorphic transformation of famotidine could not be detected by other spectroscopic methods. This suggests that the DSC heating system was a preferred method not only to quantitatively analyze the polymorphic transformation of famotidine but also to find a newly transitional phase of famotidine in the compressed compact.


Subject(s)
Anti-Ulcer Agents/chemistry , Famotidine/chemistry , Calorimetry, Differential Scanning , Pressure , Technology, Pharmaceutical
12.
Article in English | MEDLINE | ID: mdl-17703671

ABSTRACT

Sound-velocity inhomogeneities degrade both the spatial resolution and the contrast in diagnostic ultrasound. We previously proposed an adaptive imaging approach based on the coherence of the data received in the channels of a transducer array, and we tested it on phantom data. In this study, the approach was tested on clinical breast data and compared with a correlation-based method that has been widely reported in the literature. The main limitations of the correlation-based method in ultrasonic breast imaging are the use of a near-field, phase-screen model and the integration errors due to the lack of a two-dimensional (2-D) array. In contrast, the proposed coherence-based method adaptively weights each image pixel based on the coherence of the receive-channel data. It does not make any assumption about the source of the focusing errors and has been shown to be effective using 1-D arrays. This study tested its in vivo performance using clinical breast data acquired by a programmable system with a 5 MHz, 128-channel linear array. Twenty-five cases (6 fibroadenomas, 10 carcinomas, 6 cysts, and 3 abscesses) were investigated. Relative to nonweighted imaging, the average improvements in the contrast ratio and contrast-to-noise ratio for the coherence-based method were 8.57 dB and 23.2%, respectively. The corresponding improvements when using the correlation-based method were only 0.42 dB and 3.35%. In an investigated milk-of-calcium case, the improvement in the contrast was 4.47 dB and the axial and lateral dimensions of the object were reduced from 0.39 to 0.32 mm and from 0.51 to 0.43 mm, respectively. These results demonstrate the efficacy of the coherence-based method for clinical ultrasonic breast imaging using 1-D arrays.


Subject(s)
Breast Diseases/diagnostic imaging , Image Enhancement/methods , Ultrasonography, Mammary/methods , Adult , Aged , Aged, 80 and over , Algorithms , Artifacts , Feedback , Female , Humans , Middle Aged , Quality Control , Scattering, Radiation , Sensitivity and Specificity , Stochastic Processes , Transducers , Ultrasonography, Mammary/instrumentation
13.
Microsc Microanal ; 13(2): 128-32, 2007 Apr.
Article in English | MEDLINE | ID: mdl-17367552

ABSTRACT

beta-carotene was first identified from the vitreous asteroid bodies (ABs) excised from one patient with asteroid hyalosis (AH) by confocal Raman microspectroscopy and was also verified by high performance liquid chromatography (HPLC). Two patients had been diagnosed with AH and intervened by surgical vitrectomy due to blurred vision. The morphology and components of both AB specimens were observed by optical microscopy and determined by using confocal Raman microspectroscopy and HPLC analysis, respectively. Surprisingly, two unique peaks at 1528 and 1157 cm(-1) were found in the Raman spectrum for the AB specimen of patient 1 alone, which were in close agreement with that of the Raman peaks at 1525 and 1158 cm(-1) for beta-carotene and/or lutein. However, HPLC analytical data clearly indicated that the retention time for the extracted sample from the AB specimen of patient 1 was observed at 13.685 min and just identical to that of beta-carotene (13.759 min) rather than lutein (2.978 min). In addition, the lack of any peak in the HPLC profile for the AB specimen of patient 2 also confirmed the absence of Raman peaks at 1525 and 1158 cm(-1). Thus this preliminary study strongly suggests that beta-carotene as a unique component of ABs was specifically detected from the AB specimen of one AH patient by using confocal Raman microspectroscopy and HPLC analysis.


Subject(s)
Eye Diseases/metabolism , Vitreous Body/chemistry , beta Carotene/analysis , Aged , Aged, 80 and over , Chromatography, High Pressure Liquid , Eye Diseases/pathology , Eye Diseases/surgery , Female , Humans , Male , Spectrum Analysis, Raman , Vitrectomy , Vitreous Body/pathology , Vitreous Body/surgery
14.
Acta Pharmacol Sin ; 28(3): 446-52, 2007 Mar.
Article in English | MEDLINE | ID: mdl-17303010

ABSTRACT

AIM: To study the effect of gum mastic, a natural resin, on the proliferation of androgen-independent prostate cancer PC-3 cells, and further investigate the mechanisms involved in this regulatory system, taking nuclear factor kappaB (NF-kappaB) signal as the target. METHODS: 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay and a flow cytometer were used to detect the effect of gum mastic on the proliferation of PC-3 cells. Then, reporter gene assay, RT-PCR, and Western blotting were carried out to study the effects of gum mastic on the NF-kappaB protein level and the NF-kappaB signal pathway. The expression of genes involved in the NF-kappaB signal pathway, including cyclin D1, inhibitors of kappaBs (I kappaB alpha), and phosphorylated Akt (p-AKT), were measured. In addition, transient transfection assays with the 5X NF-kappaB consensus sequence promoter was also used to test the effects of gum mastic. RESULTS: Gum mastic inhibited PC-3 cell growth and blocked the PC-3 cell cycle in the G1 phase. Gum mastic also suppressed NF-kappaB activity in the PC-3 cells. The expression of cyclin D1, a crucial cell cycle regulator and an NF-kappaB downstream target gene, was reduced as well. Moreover, gum mastic decreased the p-AKT protein level and increased the I kappa B alpha protein level. CONCLUSION: Gum mastic inhibited the proliferation and blocked the cell cycle progression in PC-3 cells by suppressing NF-kappaB activity and the NF-kappaB signal pathway.


Subject(s)
Antineoplastic Agents, Phytogenic/pharmacology , NF-kappa B/drug effects , Prostatic Neoplasms/drug therapy , Resins, Plant/pharmacology , Androgens/physiology , Cell Nucleus/chemistry , Cell Nucleus/metabolism , Cell Proliferation/drug effects , Cyclin D1/biosynthesis , Cyclin D1/genetics , Humans , Male , Mastic Resin , Oncogene Protein v-akt/biosynthesis , Oncogene Protein v-akt/genetics , Reverse Transcriptase Polymerase Chain Reaction , Signal Transduction/drug effects
15.
Article in English | MEDLINE | ID: mdl-17225801

ABSTRACT

Most conventional blood flow estimation methods measure only the axial component of the blood velocity vector. In this study, we developed a new method for two-dimensional (2-D) velocity vector estimation in which time shifts resulting from blood motion are calculated for the individual channels using aperture domain data. This allows the construction of a time-shift profile along the array direction as a function of channel index, which is approximated by a first-order polynomial whose zeroth-order and first-order terms can be used to determine the axial and lateral velocity components, respectively. The efficacy of the proposed method was verified by simulations and experiments in which the transducer array had 64 elements, an aperture size of 1.96 cm, and a center frequency of 5 MHz. The flow velocity ranged from 5 to 35 cm/s and the Doppler angle ranged from 0 degrees to 90 degrees. The experimental results show that the accuracy of axial velocity estimation is higher for the new method than for the autocorrelation-based conventional method when the signal-to-noise ratio is larger than 0 dB. The mean estimation error for the axial velocity component is 2.18% for the new method, compared to 4.51% for the conventional method. The mean estimation error for the lateral velocity component is 15%, which is comparable to existing methods.


Subject(s)
Algorithms , Blood Flow Velocity/physiology , Image Enhancement/methods , Image Interpretation, Computer-Assisted/methods , Rheology/methods , Ultrasonography, Doppler/methods , Information Storage and Retrieval/methods , Phantoms, Imaging , Reproducibility of Results , Sensitivity and Specificity , Ultrasonography, Doppler/instrumentation
16.
J Pharm Biomed Anal ; 43(2): 457-63, 2007 Jan 17.
Article in English | MEDLINE | ID: mdl-16934429

ABSTRACT

In order to investigate the thermal-related properties and thermal stability of 10-hydroxycamptothecin (10-HCPT) in the solid state, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) microspectroscopy were used. A novel combination of FT-IR microspectroscopy with thermal analyzer was applied simultaneously to monitor the dehydration and rehydration processes of the 10-HCPT sample. The thermal-induced decomposition of the 10-HCPT sample was also determined by using electrospray-ion trap mass spectrometry (ES-ITMS). The results indicated that the 10-HCPT sample used in this study was a monohydrate in structure, this form that can dehydrate to an anhydrate form if the temperature goes beyond 90 degrees C. The 10-HCPT anhydrate was first suggested to have two polymorphs, in which the form I might transform to form II when the 110 degrees C-preheated sample was cooled to 30 degrees C. The polymorphic transformation temperature was shown within 90-120 degrees C with 10.46 kcal/mol of enthalpy. The peak at 1723 cm(-1) found in the IR spectrum of 10-HCPT monohydrate might correspond to the hydrogen-bonded CO stretching vibration of lactone, which shifted to 1750 cm(-1) assigned to a free CO group of lactone after the destruction of hydrogen bonding via dehydration. This suggests that monohydrate seems to interact intramolecularly with 10-HCPT by hydrogen bonding. However, the rehydration process of the 10-HCPT anhydrate might cause it to return to being a monohydrate, depending on the storage condition. In addition, the thermal-induced decarboxylation of the solid-state 10-HCPT when the temperature is beyond 226 degrees C was proven by the appearance of a new IR peak at 1701 cm(-1) and one major mass spectral peak at m/z 321. This unique IR spectral peak at 1701 cm(-1) was due to the conjugated carbonyl group in the degraded product of 10-HCPT. The m/z 321 assigned to the decarboxylation of 10-HCPT was equal to the molecular weight loss of 44 from mass spectra; which was consistent with the weight loss of 11.9% (molecular weight of 43.3) from TGA curve of 10-HCPT anhydrate.


Subject(s)
Antineoplastic Agents, Phytogenic/chemistry , Camptothecin/analogs & derivatives , Calorimetry, Differential Scanning , Camptothecin/chemistry , Decarboxylation , Desiccation , Drug Stability , Hydrogen Bonding , Microspectrophotometry , Molecular Structure , Spectrometry, Mass, Electrospray Ionization , Spectroscopy, Fourier Transform Infrared , Temperature , Thermodynamics , Thermogravimetry , Water/chemistry
17.
Int J Pharm ; 318(1-2): 86-91, 2006 Aug 02.
Article in English | MEDLINE | ID: mdl-16647827

ABSTRACT

Two polymorphs of famotidine were prepared by recrystallization from acetonitrile for form A and methanol for form B, respectively. The effect of grinding process on the polymorphic transformation of famotidine was investigated. Each famotidine sample ground for various grinding times in a ceramic mortar was determined by differential scanning calorimetry (DSC), conventional and thermal Fourier transform infrared (FT-IR) microspectroscopy. The results indicate that the raw material of famotidine was proved to be a form B. A unique IR absorption band at 3505 cm(-1) for famotidine form B gradually decreased its intensity with the grinding time, while two newer IR absorption bands at 3451 and 1671 cm(-1) for famotidine form A slowly appeared. The peak intensity ratio of 3451/350 5 cm(-1) was linearly (r=0.9901) increased with the grinding time, suggesting that the grinding process could induce the polymorphic transformation of famotidine from form B to form A by a zero-order process. The DSC endothermic peaks also confirmed this polymorphic transformation from famotidine form B (167 degrees C, DeltaH: 165J/g) to famotidine form A (174 degrees C, DeltaH: 148J/g) in which the values of enthalpy were linearly reduced with the increase of grinding time (r=0.9943). The phase transition temperature of the different ground famotidine samples could be easily and only evidenced by using thermal FT-IR microspectroscopy, rather than by DSC analysis. These phase transition temperatures of the famotidine form B ground for 5-20 min quickly reduced from 144 to 134 degrees C and maintained a constant at 134 degrees C even after 20-30 min grinding. The grinding process not only decreased the crystallinity of famotidine form B but also reduced the particle size of famotidine form B, resulting in easy induction of the polymorphic transformation of famotidine from form B to form A in ground famotidine sample.


Subject(s)
Famotidine/chemistry , Histamine H2 Antagonists/chemistry , Calorimetry, Differential Scanning , Chemical Phenomena , Chemistry, Pharmaceutical , Chemistry, Physical , Drug Compounding , Excipients , Isomerism , Kinetics , Particle Size , Spectroscopy, Fourier Transform Infrared , Thermodynamics
18.
Biophys Chem ; 114(2-3): 205-12, 2005 Apr 22.
Article in English | MEDLINE | ID: mdl-15829354

ABSTRACT

In order to investigate the thermal stability of human serum albumin (HAS) in three different states (aqueous solution, cast film, and solid powder), Fourier transform infrared (FTIR) spectroscopy was applied to determine the protein secondary structural changes of these HSA samples under non-isothermal or isothermal condition. The structural similarity of HSA before and after thermal treatment was also studied to estimate the thermo-reversible property of the HSA in these different states. The results indicate that with the increase of temperature, the maximum peaks at 1652 and 1547 cm(-1) (alpha-helix) shifted to 1647 and 1542 cm(-1) (random coil), respectively. An additional peak at 1620 cm(-1) assigned to intermolecular beta-sheet structure clearly appeared with temperature. The alpha-helix content was found to be reduced in favor of the formation of intermolecular hydrogen-bonded antiparallel beta-sheet structure beyond 60 degrees C in the heating process. From the data of structural similarity, HSA sample whether in solid powder or cast film form exhibited a better thermo-reversible property than HSA in aqueous solution even heating to 200 degrees C.


Subject(s)
Serum Albumin/chemistry , Drug Stability , Humans , Membranes, Artificial , Powders/chemistry , Solutions/chemistry , Temperature , Thermodynamics
19.
Pharm Res ; 21(11): 2127-32, 2004 Nov.
Article in English | MEDLINE | ID: mdl-15587937

ABSTRACT

PURPOSE: Enalapril may undergo the thermal-induced intramolecular interaction to cause an enalapril diketopiperazine (DKP) formation. It is interesting to study the influence of Eudragit E, as a coating polymer, on the stability of enalapril maleate. The reaction kinetics of the solid-state degradation process of pure enalapril maleate and Eudragit E/enalapril maleate mixture with different weight ratios were examined. The mechanism of solid-state interaction between Eudragit E and enalapril maleate was also discussed. METHODS: The cast samples of pure enalapril maleate or Eudragit E/enalapril maleate mixture after evaporating the solvent were prepared on an aluminum foil and also determined by reflectance Fourier transform infrared (FTIR) microspectroscopy equipped with thermal analyzer. RESULTS: The result indicates that the interaction might occur between enalapril maleate and Eudragit E in the solid state after evaporating the solvent. The thermal-dependent FTIR spectra show that not only the formation of DKP but also the six-membered cyclic anhydride occurred in the enalapril maleate/Eudragit E mixture in the heating process. Two pathways for solid-sate interaction were proposed. The stability of enalapril maleate was dependent on the weight ratio of enalapril maleate and Eudragit E. The activation energy (n = 3) of DKP formation for pure enalapril maleate was about 141.2+/-0.7 kJ/mol, but it was reduced significantly to 86.7+/-0.8 kJ/mol after interaction with Eudragit E (weight ratio: 1:1), suggesting Eudragit E might exacerbate the degradation of enalapril maleate. However, the degradation accelerated by Eudragit E was reduced in high content of Eudragit E. CONCLUSIONS: When the weight ratio of both components was 1:1, Eudragit E might interact with the carboxyl group of maleic acid to exacerbate the degradation of enalapril maleate. However, the excess amount of Eudragit E might somewhat reduce the degradation of enalapril, due to the interaction that occurred between Eudragit E and carboxyl group of enalapril.


Subject(s)
Angiotensin-Converting Enzyme Inhibitors/metabolism , Enalapril/metabolism , Methacrylates/pharmacology , Piperazines/metabolism , Algorithms , Diketopiperazines , Excipients/pharmacology , Kinetics , Maleates/metabolism , Methylmethacrylates , Spectroscopy, Fourier Transform Infrared
20.
J Biomed Mater Res B Appl Biomater ; 70(2): 203-8, 2004 Aug 15.
Article in English | MEDLINE | ID: mdl-15264301

ABSTRACT

Fourier-transform infrared (FTIR) microspectroscopy combining with attenuated total reflection (ATR) microsampling technique and micro-Raman spectrophotometer were used to detect the deposited materials on the surface of acrylic hydrogel intraocular lens (IOL) with or without ocular implantation. Surface morphology and the interface of this IOL were further examined by a confocal laser scanning microscope. The brand-new IOL exhibited a very smooth, transparent and featureless surface, but the explanted IOL had an irregular cerebriform-like opaque appearance. Both FTIR/ATR and Raman microspectroscopic analyses showed the deposits on the surface of acrylic hydrogel IOL after ocular implantation to consist of octacalcium phosphate (OCP) and Type B carbonated apatites, leading to the opalescence of acrylic hydrogel IOL. Both vibrational microspectroscopic examinations also confirmed the mineralization still in progress on the surface of acrylic hydrogel IOL after ocular implantation for 2 years.


Subject(s)
Apatites/chemistry , Calcium Phosphates/chemistry , Lenses, Intraocular , Aged , Humans , Hydrogels , Male , Microscopy, Confocal , Spectroscopy, Fourier Transform Infrared , Spectrum Analysis, Raman
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