ZEB2 knockdown inhibits interleukin-1ß-induced cartilage degradation and inflammatory response through the Wnt/ß-catenin pathway in human chondrocytes.

OBJECTIVE: Osteoarthritis (OA) is a degenerative disease of the joints characterized by inflammation and cartilage degeneration. Zinc finger E-box binding homeobox 2 (ZEB2) contains various function domains that interact with multiple transcription factors involved in various cellular functions. However, the function of ZEB2 in OA has not been clearly illustrated. METHOD: Interleukin-1ß (IL-1ß) was used to establish an OA model in vitro. We quantified the ZEB2 expression in cartilage tissues from OA patients and IL-1ß-induced chondrocytes through reverse transcription-quantitative polymerase chain reaction and Western blot. We then used functional assays to explore the function of ZEB2 during OA progression. RESULTS: ZEB2 expression was increased in OA cartilage tissues and chondrocytes. The silencing of ZEB2 increased aggrecan and collagen II levels, and reduced the content of matrix metalloproteinase-3 (MMP-3), MMP-9, and MMP-13. ZEB2 knockdown inhibited the effects of IL-1ß on the production of nitric oxide and prostaglandin E2, and the expression of inducible nitric oxide synthase and cyclooxygenase-2. ZEB2 inhibition also suppressed the levels of IL-6 and tumour necrosis factor-α, and increased the IL-10 level in IL-1ß-treated cells. Mechanically, ZEB2 knockdown blocked the activation of the Wnt/ß-catenin pathway in chondrocytes. CONCLUSION: Knockdown of ZEB2 alleviated IL-1ß-induced cartilage degradation and the inflammatory response through the Wnt/ß-catenin pathway in chondrocytes.

[Effect of various intracanal materials on the diagnostic accuracy of cone-beam computed tomography in vertical root fractures].

OBJECTIVE: To study the effect of various intracanal materials on the accuracy of oral maxillofacial cone-beam computed tomography (CBCT) for the diagnosis of vertical root fracture (VRF). METHODS: A total of twenty-four structurally intact single root canal dried and isolated teeth extracted for orthodontic treatment or periodontal disease were collected. The teeth were decrowned along the cemento-enamel junction (CEJ) and then used as samples for the study after conventional root canal preparation and post preparation. The 24 samples were divided into two groups with 12 samples in each group. Group A was the control group (no VRF group). According to intracanal materials, they were divided into five subgroups: blank group, fiber post group, gutta-percha point group, titanium post group and gold-palladium post group. Group B was the experimental group (VRF group), and subgroups were grouped as above. The VRF model was prepared by a unified method in the VRF group: the root was completely fractured in the buccolingual direction with a custom root canal nail and then cemented and reset. The control group was not subjected to the simulation of VRF. Titanium post and gold-palladium post were made according to the individuality of the root canal preparation, and the tightness of the post to the root canal wall was confirmed by X-ray radiograph. Then all the samples were scanned by CBCT in the isolate swine mandibular alveolar sockets. The diagnostic accuracy was statistically analyzed via blind interpretation by experienced endodontic specialists and oral and maxillofacial medical imaging specialists. RESULTS: The accuracy of the diagnosis of VRF in the blank group, fiber post group, gutta-percha point group, titanium post group, and gold-palladium post group in CBCT was 95.83%, 91.67%, 87.50%, 79.17%, and 45.83%, respectively. Compared with the blank group, the differences were not statistically significant in the fiber post group (P>0.999), the gutta-percha point group (P=0.500) and the titanium post group (P=0.125). The lowest diagnostic accuracy of VRF was found in the gold-palladium post group, and the difference was statistically significant compared with all other groups (P < 0.001). CONCLUSION: Various intracanal materials have different degrees of influence on the diagnostic accuracy of VRF diagnosis in CBCT. The influence of fiber post, gutta-percha point and titanium post was small, while the influence of gold-palladium post was significant.

Performance of the BL03U beamline at SSRF.

The vacuum ultraviolet beamline BL03U with a photon energy range from 7 eV upwards has been constructed at the 3.5 GeV Shanghai Synchrotron Radiation Facility. Equipped with an APPLE-Knot undulator, this beamline is dedicated to angle-resolved photoemission spectroscopy. An energy-resolving power of higher than 4.6 × 104 has been achieved in the photon energy range 21.6-48 eV, which is almost the same as the theoretical estimation.

[Measurement of the weight and volume of submandibular gland in vitro].

OBJECTIVE: To measure the weight and volume of normal submandibular gland by in vitro detection of glandular body, to compare with the measurement values of CT volume rendering to evaluate the consistency of the two methods, and to explore the related factors affecting the weight and volume of the submandibular gland. METHODS: The patients who underwent neck dissection due to oral cancer and were confirmed with normal submandibular gland by postoperative histopathology in Peking University School and Hospital of Stomatology from May 2019 to January 2020 were collected in this study and divi-ded into 4 groups according to the age standards raised by the Society of Geriatrics Chinese Medical Association and WHO (2000) age standards. The submandibular gland was carefully dissected along with the capsule immediately after neck dissection. The weight and volume of submandibular gland were accurately measured by an integrated aseptic measuring device. The volume of submandibular gland was measured by CT volume rendering before operation and the consistency of the two methods was evaluated. The 95% confidence interval of the weight and volume of submandibular gland in the different groups of Chinese people, which were divided by gender and age, were calculated, and the correlation with age, gender, height, weight, body mass index (BMI) and other factors was analyzed. RESULTS: The weight and vo-lume of submandibular gland were measured in 220 subjects. The average weight and volume of submandibular gland were (11.69±2.45) g and (11.55±2.41) cm3 respectively. The volume of submandibular gland measured by CT volume rendering ranged from 70% to 82% of that measured by in vitro detection of glandular body, and the correlation coefficient between the two methods was 0.976 (P < 0.05). The gender difference of weight and volume of submandibular gland existed in the groups of youth, middle-aged, young elderly and elderly groups, the values of males were obviously higher than those of females (P < 0.05). There was no gender difference of weight and volume of submandibular gland in the adolescent group (P > 0.05). The weight and volume of submandibular gland had a strong positive correlation with body height (P < 0.05), a weak positive correlation with body weight (P < 0.05), and no correlation with BMI (P > 0.05). The female's weight and volume of submandibular gland in the young elderly and elderly groups were significantly lower than those in the other three groups (P < 0.05). CONCLUSION: The normal reference range of the weight and volume of submandibular gland in vitro were established in different age and gender groups of Chinese people. The volume of submandibular gland mea-sured by CT volume rendering was 70%-82% of that measured by in vitro detection of glandular body. The results of the two methods had a high degree of consistency. The weight and volume of submandibular gland were related to age, gender, body height and body weight.

[Parotid CT imaging reporting and data system: A preliminary study].

OBJECTIVE: To establish a Parotid Imaging Reporting and Data System (PI-RADS) for CT diagnosis of the parotid gland neoplasms and to investigate the clinical applicable value and feasibility of PI-RADS. METHODS: Patients who had been diagnosed with primary parotid gland neoplasms and had received surgical treatments in Peking University School and Hospital of Stomatology during the period of January 2013 to December 2016 were included in this study. The diagnoses were confirmed by the postoperative pathological examinations in all the patients. The CT imaging data of all patients were retrospectively reviewed and analyzed by two readers in consensus. Imaging characteristics related to the parotid neoplasms were extracted and quantified. Based on comprehensive analysis of the imaging characteristics, the probabilities of the benign and malignant neoplasms were evaluated and classified into six grades, PI-RADS 1-6 (PI-RADS 1: normal parotid gland; PI-RADS 2: confidently benign lesions; PI-RADS 3: probably benign lesions without confirmed evidence of malignancy; PI-RADS 4: suspected malignancy without sufficient evidence of malignancy; PI-RADS 5: confidently malignant lesions; PI-RADS 6: lesions with confirmed pathological evidence of malignancy). RESULTS: A total of 897 patients with 1 003 parotid lesions were included. The lesions included 905 benign and 98 malignant lesions. The proportions of the malignancies in PI-RADS 2, PI-RADS 3, PI-RADS 4 and PI-RADS 5 according to the two readers in consensus were 0.4%, 5.7%, 35.5% and 96.7% respectively. The overall Cohen's Kappa test showed medium consistency between the two independent researchers (κ=0.614, P<0.001, 95%CI: 0.569-0.695). Pearson Chi-square test showed that the proportions of malignancies increased with the diagnostic PI-RADS grades (Cochran-Armitage trend test, Z=-15.579, P<0.001). The results of Pearson Chi-square tests showed significant differences between the grades [PI-RADS 2 and 3 (χ²=12.048, P=0.001); PI-RADS 3 and 4 (χ²=75.231, P<0.001); PI-RADS 4 and 5 (χ²=32.266, P<0.001)]. CONCLUSION: PI-RADS can be used to evaluate the risk of malignancy and will be helpful to improve the imaging diagnosis and clinical treatment of parotid gland neoplasms.

[Computed tomographic features of desmoplastic ameloblastoma of the jaw].

OBJECTIVE: To retrospectively analyze the clinical and CT imaging features of desmoplastic ameloblastomas (DA) in comparison with other types of ameloblastomas. METHODS: Patients diagnosed with ameloblastoma histopathologically in Peking University School and Hospital of Stomatology from July 2000 to August 2017 were reviewed to analyze the constituent ratios and characteristics of DA. CT imaging features of DA (28 cases) were investigated in comparison with consecutive cases of solid/multicystic and unicystic ameloblastomas. The following imaging perspectives were analyzed: the border, internal structure, three-dimensional shape, tooth, the periodontium, the cortex and the expansion of the tumors. CT values were measured in the region of interest for quantitative analysis. RESULTS: Among the 1 269 cases of ameloblastomas, 50 (3.9%) were DA, which showed predilections for males (74.0%). The average age of DA was about 43.9 years old, which was higher than the other two types. The anterior incisorcanine region (62.0%) and premolar region (30.0%) were most frequently affected. The incidence rate of DA in mandibule was 56.0% (28/50), which was slightly higher than that of maxilla (44.0%). The DA characteristically showed scallop border and honeycomblike or soapbubble internal structure with bone formation on CT. The mean ratios of height to mesiodistal and buccal-lingual to mesio-distal distances were 0.76 and 0.63, which were higher than the other two types. According to the degree of internal bone formation, three subtypes of DA could be observed: densely ossifying type (I), honeycomb/soap bubble type (II) and sparsely ossifying type (III). The means and standard deviations of CT values of DA were significantly higher than those of the other two types, which were (488.8±164.0) HU (type I), (171.7±102.8) HU (type II), (42.1±8.8) HU (type III). CONCLUSION: CT is helpful for diagnosis of DA, which shows as solid tumor with varying degrees of internal ossification.

[Clinicopathological characteristics and diagnosis of IgG4related sialadenitis].

Immunoglobulin G4-related sialadenitis (IgG4-RS) is a newly recognized immune-mediated disease and one of immunoglobulin G4-related diseases (IgG4-RD). Our multidisciplinary research group investigated the clinicopathological characteristics and diagnosis of IgG4-RS during the past 10 years. Clinically, it showed multiple bilateral enlargement of major salivary glands (including sublingual and accessory parotid glands) and lacrimal glands. The comorbid diseases of head and neck region including rhinosinusitis, allergic rhinitis, and lymphadenopathy were commonly seen, which could occur more early than enlargement of major salivary glands. Internal organ involvements, such as autoimmune pancreatitis, sclerosing cholangitis, and interstitial pneumonia could also be seen. Thirty-five (38.5%) patients had the symptom of xerostomia. Saliva flow at rest was lower than normal. Secretory function was reduced more severely in the submandibular glands than in the parotid glands. Serum levels of IgG4 were elevated in almost all the cases and the majority of the patients had increased IgE levels. CT, ultrasonography, and sialography showed their imaging characteristics. Histologically it showed marked lymphoplasmacytic inflammation, large irregular lymphoid follicles with expanded germinal centers, prominent cellular interlobular fibrosis, eosinophil infiltration, and obliterative phlebitis. Their immunohistological examination showed marked IgG-positive and IgG4-positive plasma cell infiltration and high IgG4/IgG ratio. The disease could be divided into three stages according to severity of glandular fibrosis. The serum IgG4 level was higher and the saliva secretion lower as glandular fibrosis increased. IgG4-RS should be differentiated from other diseases with enlargement of major salivary gland and lacrimal gland, such as primary Sjögren syndrome, chronic obstructive submandibular sialadenitis, and eosinophilic hyperplastic lymphogranuloma.

Clinical features of tumours and tumour-like pathologies involving the buccal fat pad.

This study aimed to investigate the clinical, radiological, and pathological characteristics of pathologies involving the buccal fat pad (BFP) and to explore the treatment protocols. The cases of 109 patients with primary pathologies involving the BFP (pBFP) diagnosed between January 2013 and September 2021 were assessed. The patients' clinical presentations and radiological and histopathological findings were analysed retrospectively, and their treatment outcomes were evaluated. The 109 pBFP were categorized as benign tumours (n = 17), malignant tumours (n = 29), vascular malformations (n = 38), and inflammatory masses (n = 25). Of the 17 benign tumours, seven were lipomas, five were pleomorphic adenomas, three were solitary fibrous tumours, and two were other tumours. The 29 malignant tumours included five adenoid cystic carcinomas, six mucoepidermoid carcinomas, three synovial sarcomas, and 15 other tumours. Of the 38 vascular malformations, 37 were venous and one was arteriovenous. Regarding the inflammatory masses, the lesions appeared after cosmetic facial botulinum toxin injection in 13 cases and after other cosmetic facial procedures in five. The upper body of the BFP was the most frequently involved site (79/109), while other frequently involved sites were the lower body (67/109) and the masseteric (41/109), temporal (32/109), and pterygopalatine (30/109) extensions.

Natural course of severe temporomandibular joint osteoarthrosis evaluated by a novel condylar remodelling scoring system and quantitative volumetric analysis.

Temporomandibular joint osteoarthrosis (TMJ-OA) frequently causes mild, moderate, or severe condylar morphological changes. A novel condylar remodelling scoring system (CRSS) based on three-dimensional cone beam computed tomography images is proposed, which is used to grade condylar morphological changes. In the CRSS, the condyle is divided into 10 regions by 11 reference points. For each increase in the number of regions involved in TMJ-OA, one point is subtracted from the full score of 10. The intra-class correlation coefficients for intra- and inter-observer agreement (range 0.656-0.898 and 0.841-0.906, respectively) indicated that the CRSS had good reliability. Cephalometric analysis showed that the condyles with severe morphological changes were prone to present with a retrognathic and clockwise rotating mandible, shorter ramus height, reduced mandibular length, larger mandibular angle, and maxillary retrusion. Qualitative CRSS evaluation and quantitative volumetric analysis were performed to evaluate the stability of severe TMJ-OA in its natural course (343 condyles). The continuous cortex group showed no remarkable changes with an average follow-up of 2 years. In the discontinuous cortex group, most (74.4%) converted into a continuous cortex during follow-up (mean 2 years).

Differential diagnosis of immunoglobulin G4-related sialadenitis and Kimura's disease of the salivary gland: a comparative case series.

The aim of this study was to investigate key points for the differential diagnosis of immunoglobulin G4-related sialadenitis (IgG4-RS) and Kimura's disease (KD) involving the salivary glands. The clinical, serological, radiological, histological, and immunohistochemical features of 85 IgG4-RS cases and 52 KD cases were evaluated comparatively. Seventy-two IgG4-RS cases had enlargement of multiple salivary and/or lacrimal glands; 67 patients had bilateral submandibular gland (SMG) involvement. Unilateral parotid gland involvement (59.6%) and comorbid skin lesions (61.5%) were common in KD. Serum IgG4 was elevated in 94.1% of IgG4-RS cases versus 19.0% of KD cases (cut-off value=266.5mg/dl). KD was more commonly associated with elevated eosinophil counts (86% vs 23.1%) and elevated IgE concentrations (95.5% vs 76.6%). Storiform fibrosis, irregular lymphoid follicles, and increased IgG4-positive cells (112.9±37.6/high-power field (HPF)) were common in IgG4-RS. Acellular fibrosis, regular lymphoid follicles, IgE-positive reticular networks, increased IgE-positive cells (43.4±26.7/HPF), and tryptase-positive mast cells (29.7±13.3/HPF) were usually detected in KD. Computed tomography showed that 85.7% of KD cases involved subcutaneous fat tissue. A superficial hypoechoic and reticular pattern with multiple hypoechoic foci were the sonographic features of the SMG in IgG4-RS. Despite numerous overlapping manifestations, histopathological examination showed meaningful differences in the types of fibrosis, eosinophils, and IgG4-positive cell counts. Comprehensive evaluation of clinical, serological, radiological, and histopathological features are crucial for the differential diagnosis.

Surgical resection of clinically benign tumours in the maxillomandibular deep lobe of the parotid gland via sternocleidomastoid muscle-parotid space approach.

This article reports the surgical resection of clinically benign tumours in the maxillomandibular deep lobe of the parotid gland via sternocleidomastoid muscle-parotid space (SPS) approach. The use of maxillary-mandibular planes to subdivide the deep lobe of the parotid gland in order to establish the tumour location and accessibility is introduced. This approach, which does not raise a skin flap, may preserve the superficial lobe. Ten patients with clinically benign tumours in the maxillomandibular deep lobe of the parotid gland were treated via the SPS approach. The patients were followed up for 3-5 years and the surgical outcomes were analysed. All tumours were completely enucleated via the SPS approach with an optimal aesthetic outcome. No permanent facial weakness or tumour recurrence was identified during the 3-5 years of follow-up. The SPS approach to surgical resection is an ideal option for clinically benign tumours in the maxillomandibular deep lobe of the parotid gland and demonstrates good results.

Banded surface flow maintained by convection in a model of the rapidly rotating giant planets.

In three-dimensional numerical simulations of a rapidly rotating Boussinesq fluid shell, thermally driven convection in the form of columns parallel to the rotation axis generates an alternately directed mean zonal flow with a cylindrical structure. The mean structure at the outer spherical surface consists of a broad eastward flow at the equator and alternating bands of westward and eastward flows at higher latitudes in both hemispheres. The banded structure persists even though the underlying convective motions are time-dependent. These results, although still far from the actual motions seen on Jupiter and Saturn, provide support for theoretical suggestions that thermal convection can account for the remarkable banded flow structures on these planets.

Distribution of Ca2+-activated K+ channel isoforms along the tonotopic gradient of the chicken's cochlea.

In some cochleae, the number and kinetic properties of Ca2+-activated K+ (KCa) channels partly determine the characteristic frequency of each hair cell and thus help establish a tonotopic map. In the chicken's basilar papilla, we found numerous isoforms of KCa channels generated by alternative mRNA splicing at seven sites in a single gene, cSlo. In situ polymerase chain reactions demonstrated cSlo expression in hair cells and revealed differential distributions of KCa channel isoforms along the basilar papilla. Analysis of single hair cells by the reverse transcription polymerase chain reaction confirmed the differential expression of channel variants. Heterologously expressed cSlo variants differed in their sensitivities to Ca2+ and voltage, suggesting that the distinct spatial distributions of cSlo variants help determine the tonotopic map.

Exposure of residues in the cyclic nucleotide-gated channel pore: P region structure and function in gating.

In voltage-gated ion channels and in the homologous cyclic nucleotide-gated (CNG) channels, the loop between the S5 and S6 transmembrane segments (P region) is thought to form the lining of the pore. To investigate the structure and the role in gating of the P region of the bovine retinal CNG channel, we determined the accessibility of 11 cysteine-substituted P region residues to small, charged sulfhydryl reagents applied to the inside and outside of membrane patches in the open and closed states of the channel. The results suggest that the P region forms a loop that extends toward the central axis of the channel, analogous to the L3 loop of bacterial porin channels. Furthermore, the P region, in addition to forming the ion selectivity filter, functions as the channel gate, the structure of which changes when the channel opens.

Prognostic factors in mandibular gingival squamous cell carcinoma: A 10-year retrospective study.

The mandibular gingiva is the second most common site of oral cavity squamous cell carcinoma. This retrospective study was designed to determine the clinicopathological features of squamous cell carcinoma of the mandibular gingiva (MGSCC) and to establish a new risk model to predict overall survival. The study included 207 patients with primary MGSCC from January 2000 to September 2009. The medical charts were reviewed and data related to clinical characteristics, treatment provided, histopathological analysis, and follow-up were recorded. All patients underwent surgery as the first-line therapy; follow-up ranged from 1 to 171 months (median 63 months). Clinical characteristics and pathological outcomes were analyzed with respect to the 5-year overall survival rate. A survival risk model was established, and patients were classified into low-, moderate-, and high-risk groups based on the prognostic index designed in this study. The 5-year overall survival rates for the low-, moderate-, and high-risk groups were 92.3%, 76.9%, and 34.2%, respectively. Pathological node metastasis, perineural invasion, and extracapsular spread were the most significant predictive factors for 5-year overall survival. MGSCC is not aggressive, and the survival outcomes of MGSCC are better than those of squamous cell carcinoma (SCC) at other sites. It is suggested that patients with T2-T4 tumours undergo elective neck dissection and those with T1 tumours be followed up without addressing the neck.

[The effects of pressure controlled ventilation for tracheobronchial foreign body removal in children].

Objective:To evaluate the effects of pressure controlled ventilation for tracheobronchial foreign body removal in children.Method: Ninety ASAⅡor Ⅲ children,aged 10 months to 3 yr,weighing 8-16 kg undergoing removal of airway foreign body were randomly divided into 3 groups(n=30 each):groupⅠpressure controlled ventilation(P)，group Ⅱ high-frequency jet ventilation(H),and group Ⅲ, reserve spontaneously breathings.Arterial blood gas analysis of Pre-operation and the end of operation,the occurrence of hypoxia during operation,the duration of operation,anesthesia emergence time and perioperative side effects were recorded. Result:The arterial blood gas analysis(PaO2,PaCO2,SaO2)and SPO2of Pre-operation in group P and H had no significant difference. The PaO2 of the end of operations was significantly higher,and PaCO2 was lower in group H. The occurrence of hypoxia during operation, the duration of operation,anesthesia emergence time and perioperative side effects in two group had no significant difference.Conclusion:The effects of pressure controlled ventilation and high-frequency jet ventilation for tracheobronchial foreign body removal in children were nearly the same,and pressure controlled ventilation can be commonly used in clinic.

Surgical safety distances in the infratemporal fossa: three-dimensional measurement study.

The wedge-shaped infratemporal fossa is a constricted space and has long been a surgical challenge, mainly due to difficulties in access. Three-dimensional (3D) reconstruction of the skull, internal carotid artery (ICA), and internal jugular vein (IJV) was carried out using enhanced computed tomography (CT) data, to measure the safety distances in relation to infratemporal fossa surgery. Fifty enhanced CT datasets were selected to reconstruct 3D images by segmentation technique. The anatomical routes of the ICA, IJV, and the styloid process (SP) were observed. The following were measured: SP length, height of the pterygoid plates (PP height), distances from the pterygoid process (antero-inferior and anterosuperior border) to the leading edge of the ICA (PP-ICA (inferior), PP-ICA (superior)), and distance between the most prominent point of the zygomatic arch and the medial pterygoid plate (Zyg-MPP). The mean measurements of SP length, PP height, and the distances PP-ICA (inferior), PP-ICA (superior), and Zyg-MPP were 30.64 mm, 26.61 mm, 31.16 mm, 34.37 mm, and 51.37 mm, respectively. No significant differences were observed by age group, except the distance of PP-ICA (inferior) on the left side. In centres without intraoperative navigation facilities, proper knowledge of the anatomy, particularly of bony landmarks and the safe distances to nearby neurovascular structures, can provide useful information to ensure safe operations.

Micellar electrokinetic capillary chromatography theory based on conventional chromatography.

From the definitions of retention time (tR) and resolution (Rs) in conventional chromatography, two fundamental equations for the retention behaviour and resolution of neutral solutes are derived and proved to be valid in all cases of micellar electrokinetic capillary chromatography (MECC). Two parameters, phase velocity ratio (Pr) and column availability (Aco), are introduced to reveal clearly the relationships and differences between MECC and conventional chromatography. The tR and Rs values may be either positive or negative in MECC. A negative tR indicates that the solute migrates toward the positive electrode and a positive tR toward the negative electrode. Rs > 0 means that the solute with a smaller value of the capacity factor (k') in the pair of solutes reaches the detector first, while Rs < 0 means that the elution order is the opposite. MECC can be classified into eight cases depending on the values of Pr for convenience of discussion. So far, MECC was usually performed in case IV and the resolution was poorer than that in conventional chromatography for given values of theoretical plate number, selectivity and k'. However, a better resolution can be obtained in cases II, VI and VIII when Pr < (1-k')/2. Cases VI, VIII and II are preferable to case IV for high resolution and should be more frequently employed in the future.

Assay for the determination of low dosage form of formoterol dry syrup by capillary electrophoresis with head-column field-amplified sample stacking.

The development of a capillary zone electrophoresis method with head-column field-amplified sample stacking injection for the determination of formoterol (FMTR) in a low dosage dry syrup form was described. To obtain the highest sensitivity, the sample solution was prepared by high content of organic solvent with the presence of a small amount of H+ (60-100 microM) and the capillary inlet end was dipped in water before electroinjection. This method was fully validated in terms of repeatability (RSDs for migration time, peak area of FMTR and peak area ratio between FMTR and I.S. at 1 microg/ml of FMTR was 0.76, 1.10 and 0.55% respectively), reproducibility (RSDs from different capillaries, analytes, days and instruments were 1.52%, 1.04%, 1.16% and 1.93% respectively), linearity (y = 0.827x - 0.085, r = 0.9993 (n = 6) over the range of 0.25-2.0 microg/ml), limits of quantitation, ruggedness and robustness. The method was applied to the determination of the drug in commercial dry syrup preparation (recovery was 100.9%, RSD = 1.5%, n = 5) and proved to be fast and reliable for the quantitation analysis of FMTR in the pharmaceutical form.

[A new chiral derivatizing reagent for the resolution of amine and alcohol drug enantiomers by HPLC].

A new chiral derivatizing reagent (s)-alpha-methoxybenzyl isocyanate (MIB) was prepared from (s)-(+)-mandelic acid with a practical method, and its ability of liquid chromatographic resolution for drug enantiomers by pre-column chiral derivatization was evaluated with racemic amphetamine and mexiletine as well as phenylpropanol. The operation is simple and rapid. Separation is good for the amine isomers, but poor for alcohols and extensive work remains to be done. The solution of derivatization was directly injected into the chromatograph. Conventional silica gel column was used with light petroleum as the mobile phase.