The emulsification-internal gelatin method is used to formulate alginate gels and alginate-chitosan microcapsules;Diffusion properties of the alginate gels and alginate-chitosan microcapsules also were investigated with spectrophotometry by the permeability to VitaminB12.The swellability of the alginate gels and alginate-chitosan microcapsules also were investigated,and the influence of the swellability on permeability also was investigated.The results show that the permeability and swellability of alginate-chitosan microcapsules was lower than alginate gels.

A high performance liquid chromatographic method was developed for the resolution of optical isomers of beta-amino ketone compounds containing two chiral centres. An AE. Lichrom AM 1 chiral chromatographic column (250 mm x 4.6 mm, 5 microm) was used. The influences o the mobile phase polarity, flow rate and elution mode were investigated. The optimum conditions were the use of hexane-isopropyl alcohol as the mobile phase with a flow rate of 1 mL/min and gradient elution. Under the above chromatographic conditions, the optical isomers of four kinds beta-amino ketone compounds containing two chiral centres were baseline separated (Rs > 1.5). It was proved that the method is fast and easy to separate the optical isomers of beta-amino ketone compounds containing two chiral centres.

Titania-coated silica spheres were prepared by a layer-by-layer self-assembly technique for use as a high-performance liquid chromatography packing. This packing has a high surface area of 202.1 m(2)/g, a large pore volume of 0.36 cm(3)/g, and a pore diameter of 7.0 nm. Furthermore, the packing particles exhibit narrow pore size distribution and good pore structure. The chromatographic behavior of the packing was studied under both normal and reversed-phase conditions. Low column pressures were observed. Aromatic isomeric compounds were well separated on the TiO(2)/SiO(2) column under normal phase conditions; pyridine and aniline derivatives were separated on the octadecyl-bonded TiO(2)/SiO(2) (ODT) column, respectively, under reversed-phase conditions, and highly symmetrical peaks were obtained for 15 basic compounds. The chemical stability of the stationary phase was tested with sodium phosphate solution (10 mmol/L, pH = 10) at 25 degrees C and potassium phosphate solution (50 mmol/L, pH = 10) at 50 degrees C.

用通常方法制备的海藻酸钙-几丁聚糖微胶囊微粒存在着彼此粘连的问题。为此,试验了改变几丁聚糖包裹液的浓度和包裹时间等措施,效果不佳。对文献方法进行了改进,通过改变几丁聚糖包裹液的配制组成及制备微胶囊的操作步骤,有效地解决了微胶囊微粒彼此粘连的问题,制备出形状较好、离散的海藻酸钙-几丁聚糖微胶囊微粒。

A rapid, specific and highly sensitive method for the determination of seven sex hormones (norgestrel, methyltestosterone, testosterone propionate, medroxyprogesterone acetate, megestrol acetate, chlormadinone acetate, and nandrolone) residues in fish products was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization (ESI) in positive mode. The target compounds were extracted with methanol after the enzyme hydrolysis of the fish products. ZnCl2 was added to the extract solution to remove lipids. Then target compounds were purified by an LC-C18 and an LC-NH2 solid phase extraction cartridges. The target compounds were separated on a Waters ACQUITY UPLC BEH-C18 column (100 mm x 2.1 mm, 1.7 microm) and detected qualitatively and quantitatively in multi reaction monitoring (MRM) mode. For the seven sex hormones, the limits of detection (LOD) of the method were from 0.08 to 0.17 microg/kg and the limits of quantification (LOQ) were in the range of 0.24 -0.58 microg/kg. At the spiked levels of 1 and 4 microg/kg, the average recoveries ranged from 76% to 118% with the relative standard deviations between 5.0% and 11.3% for the seven sex hormones using internal standard method; and the average recoveries ranged from 66% to 94% with the relative standard deviations between 4.5% and 10.7% using matrix matched external standard method. The results showed that both methods are able to meet the multi-residue detection of the seven sex hormone residues in fish products. The degreased large yellow croaker and roast fish fillet real samples from a local market were detected by the developed method, and the seven targets were not found.

A method was developed for simultaneous determination of residues of 17 sex hormones in egg products. Target compounds were extracted from samples with methanol in an ultrasonic bath, effectively separated from lipids in the extracts by ZnCl(2) depositing filtration and purified using a C(18) solid-phase extraction (SPE) and followed by NH(2) SPE cartridge. The analytes were quantified by liquid chromatography using a BEH C(18) column coupled to an electrospray ionization tandem mass spectrometer (LC-ESI-MS/MS) operating in negative mode for estrogens and in positive multiple reaction monitoring mode for androgens. The parameters of the mass spectrometer and the composition of mobile phase and additives were also optimized to enhance detection sensitivity. Average recoveries of the target compounds varied from 70.0% to 121.0% with relative standard deviations ranging from 2.3% to 11.2% at two fortification levels. The limits of detection (LOD) of the method were from 0.002 μg kg(-1) to 0.23 μg kg(-1) and the limits of quantification (LOQ) were in the range of 0.007-0.76 μg kg(-1).

Three kinds of calcium alginate beads were prepared from three sodium alginates with different viscosities by emulsification-internal gelation.Their shapes were analyzed with a micro-analyzer and some properties of the sodium alginates were surveyed.The results showed that sodium alginate with low viscosity could be better carrier for liposoluble substances.The average diameters of the alginate beads formed from sodium alginates with differing viscosities were different.The larger the viscosity was,the larger the average diameter of the alginate beads was.

OBJECTIVE: To develop method of 7 banded synthesis sex hormones residues in egg products determined by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). METHODS: The sample were enzymolied and target compounds were extracted with methanol. ZnCl2 was added to the extract solution to remove lipid and then analytes were purified by LC-C18 and LC-NH2 solid phase extraction cartridge and further determined by UPLC-MS/MS under positive ionization and multiple reaction monitoring (MRM) modes. RESULTS: The limits of detection (LOD) of UPLC-MS/MS method used for testing Chlormadione acetate (CDA), Medroxypogesterone acetate (MPA), Megestrol Acetate (MA), Testosterone propionate (TSP), Norgestrel (NG), Methyltestosterone (MTS) and Nandrolone (NT) in egg products ranged from 0.012 to 0.23 microg/kg, and the limits of quantification (LOQ) were from 0.04 to 0.76 microg/kg. Experiments on spiked samples of egg products showed that at addition level of 2.0 microg/kg, the average recoveries of the sex hormones ranged from 80.2% to 114%, and coefficients of variation from 6.7% to 14.3%; while at addition level of 4.0 microg/kg, the average recoveries ranged from 75% to 119%, and coefficient of variation from 2.9% to 7.3%. CONCLUSION: The method could be able to identify and quantify banded synthesis hormones residues in eggs and egg products. It could be simple and sensitive, suitable for statutory residue testing.

A rapid, specific and highly sensitive multi-residue method for the determination of seven anabolic steroid residues in acidophilus milk was developed, which was based on ultra performance liquid chrmatography-electrospray tandem mass spectrometry (UPLC-MS/MS) with positive mode under multi-reaction monitoring mode. The samples were extracted with methanol under ultrasonication and purified using LC-C18 solid phase extraction cartridge. Qualitative and quantitative analysis was carried out for the analyte under the MRM mode after the separation on Waters ACQUITY UPLCTM BEH C18 (1.7 μm, 2.1×100 mm)column. The limits of detection (LOD)of the method were from 0.011 μg/kg to 0.05 μg/kg and the limits of quantification (LOQ) were in the range of 0.037~ 0.36 μg/kg. Average recoveries for the seven anabolic steroids(spiked at the levels of 0.5 μg/kg)ranged from 83%~124%,with relative standard deviations between 8.0%~24%.

Various chemical modifications of chitosan have been studied to alter their properties.This paper reported a method of modification for alginate-chitosan microcapsules with gold nanoparticles.The gold-alginate-chitosan microcapsules were prepared with gold nanoparticles solutions.Diffusion properties of the gold-alginate-chitosan and alginate-chitosan microcapsules were investigated by the permeability to Vitamin B12.And the influence of initial concentration of Vitamin B12 on permeability also was investigated in this paper.The permeability of gold-alginate-chitosan microcapsules was higher than those of before modified.And the influence of initial concentration of Vitamin B12 on permeability was paltry.

UPLC-MS/MS, a highly specific and sensitive method, was successfully developed for determining estradiol benzoate residues in infant formula milk powder.Sample preparation was involved in enzymatic digestion, extraction with methanol and clean-up by solid-phase extraction(SPE) combining C18 and NH2 columns.Estradiol benzoate was detected by ultra-performance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS) in a positive ionization mode and a multiple reaction monitoring(MRM) mode via electrospray ionization(ESI) source and quantitatively determined using nandrolone-d3 as an internal standard.The limit of detection(LOD) and limit of quantification(LOQ) using this method were 0.39 and 0.95 μg/kg for infant formula milk powder respectively.The recovery rates of estradiol benzoate spiked in infant formula milk powder at levels of 4 and 10 μg/kg were ranged from 76.5% to 86.3% with a relative standard deviations in the range of 9.7%-15.2%.

A highly sensitive ultra performance liquid chromatography/electrospray ionization tandem mass spectrometry(UPLC-MS/MS) method was developed for determination of estradiol benzoate residues in dairy products,including milk and infant formula milk powder.The sample was hydrolyzed by enzyme and extracted with methanol.The crude extract was cleaned up by solid-phase extraction(SPE) combining C18 and NH2 columns.The detection of estradiol benzoate was carried out by UPLC-MS/MS method using positive electrospray ionization(ESI+) under multiple reaction monitoring(MRM) mode.Nandrolone-d3 was used as an internal standard.Matrix-matched standards procedure was used to compensate the matrix effect.A good linearship was obtained for estradiol benzoate in the concentration range of 0.4-16 μg/kg.The limits of detection(LOD) of milk and infant formula milk powder were 0.07 μg/kg and 0.39 μg/kg,respectively,and the limits of quantification(LOQ) were 0.2 μg/kg and 0.95 μg/kg,respectively.The recoveries of estradiol benzoate spiked in milk and infant formula milk powder at the levels of 4 μg/kg and 10 μg/kg ranged from 76% to 90% with RSDs of 5.0%-15.2%.The method could meet for the requirement of estradiol benzoate residue analysis in dairy product.

Hyperbranched polymer modified carbon paste electrodes(HBP/CPF,) were prepared. The electrochemical behavior of Cu (II) on the HBP/CPE electrode was studied. In the solution of 0.25 mol/L KCI (pH 4.0), an electroactive complex of Cu (II) with poly (amine-ester) was formed and produced a redox peak at 0.27 V and 0.06 V. The HBP/CPE electrode showed good catalytic activity and sensitizing effect for the reduction of Cu (II) in the KCI solution. The investigation of the effect of structure and generation number of hyperbranched polymer on the capability of modified electrode indicates that HBP5/CPE electrode was the highest sensitizing effect. The detection limit and the linear range of the concentration of Cu(II) to the reduction peek Current were 4.0 x 10(-9) mol/L and 1.0 x 10(-9) -3.0 x 10(-5) mol/L, respectively. Linear sweep voltammetry has been applied to the determination of micro Cu (II) in human hair with satisfactory results.

The permeability is one of the most important properties of microcapsules.It is reported a modification for alginate-chitosan microcapsules with nanosized gold citrate or acrylate.The comparison of permeabilities for gold-alginate-chitosan microcapsules modified with nanosized gold citrate and acrylate was reported by spectrophotometry and using Vitamin B12 as penetrant.The experimental results showsed that the permeability of gold-alginate-chiosan microcapsules treated with citrate was higher than that of gold-alginate-chitosan microcapsules treated with acrylate.

The drawbacks of traditional drug delivery system and controlled delivery feature are reported in this present paper.Controlled drug delivery an control the administration of therapy,when medication is deployed to a targeted site through a polymeric carrier.Polysaccharides,pectin,dextran,guar gum and chitosan have been used or tested for targeted drug delivery in pharmaceutical applications.They are stable,non toxic,and enzymatically degradable in the colon.This objective is to formulate polysaccharide-based assemblies in microparticles with desirable physical and chemical properties for targeted delivery of protein drugs.Various chemical modifications of chitosan have been studied to alter their properties,including a new method of modification for alginate-chitosan microcapsules with gold nanoparticles.

A new method of modification for alginate-chitosan microcapsules with gold nanoparticles was reported. The gold-alginate-chitosan microcapsules were prepared with gold nanoparticles solutions. The optimum conditions of reactions and the particle size distributions of the gold-alginate-chitosan microcapsules were investigated. The value of pH=5.0 and reaction time of 120 minutes for reaction were chosen. The average diameters of the gold-alginate-chitosan microcapsules prepared respectively with citrate-stabilised gold nanoparticles and acrylate-stabilised gold ones were 216.686μm and 196.850 μm.

A capillary electrophoretic method for separation of the enantiomers of amlodipine in the serum of hypertension patients has been established and validated. The two enantiomers were separated in a fused-silica capillary with phosphate running buffer (75 mmol L−1, pH 2.5) containing 15 mmol L−1 hydroxypropyl-β-cyclodextrin (HP-β-CD). The effects on the separation of buffer pH and concentration, separation potential, and concentration of HP-β-CD were investigated. The range of quantitation for both enantiomers was 2.0–16.0 μg mL−1. Intra-day and inter-day relative standard deviation (RSD; n = 5) was <10%. The limits of detection (LOD) and quantification (LOQ) of the amlodipine enantiomers, at 214 nm, were approximately 0.5 and 0.7 μg mL−1, respectively (S/N = 3 and 10, respectively; 5-s injection). Recovery was always >85%. Results from enantiomer separation and quantification showed that concentrations of the enantiomers of amlodipine in serum from an elderly patient were higher than in serum from a young patient administered the same dose. The method was useful for determining the concentration of the enantiomers of amlodipine in hypertension patient serum and for monitoring the transition behavior of the enantiomers in humans. The method proved suitable for application to the separation of the enantiomers of amlodipine and analysis of clinical samples.

龙胆科植物抱茎獐牙菜Swertia franchetianaH.Smith是一种多年生草本植物,全草入药.有清热解毒、舒肝利胆之功效,主治各种肝胆疾病,临床对急性黄疸性肝炎、慢性肝炎、慢性胆囊炎等症疗效显著[1].其主要有效成分为环烯醚萜类、碳键黄酮苷类和(口山)酮苷类成分[2～5].目前,中药提取工艺筛选试验中常用化学法、生物学法及有效浸出物综合评价的方法.

A chiral stationary phase (CSP) was prepared by coating cellulose-tris(3,5-dimethylphenyl carbamate) (CDMPC) onto spherical silica gel. Four newly synthesized chiral indole derivatives were directly resolved on the CDMPC-CSP by a normal-phase system. The influences of structure and proportion of the alcohol in mobile phases on the separation by high-performance liquid chromatography with chiral stationary phase (HPLC) were investigated to optimize the chromatographic conditions. N-butano1, ethanol and ethanol were suitable for the separation of sample I, III, and IV as the modifiers, respectively, whereas the mixture of ethanol and n-propanol was suitable for sample I. Under the optimal conditions, excellent enantioseparation was achieved and the enantiomer excess values of all the four samples were determined. The satisfactory results indicated that the method of HPLC is ideal for the separation of indole derivatives.

A rapid cyclodextrin modified micellar electrokinetic chromatography (CD-MEKC) method was proposed for the determination of resibufogenin and cinobufagin in the Chinese herbal extracts from toad venom and its medicinal preparation (Liushen tablet). The two components have the close structural similarity and similar hydrophobicity, which result in poor resolution in normal MEKC. The addition of neutral beta-CD to the MEKC system was found to improve the separation of the studied compounds. The effects of several CD-MEKC parameters on the resolutions were evaluated systematically. Based on the investigation, a background electrolyte solution consisting of 10 mM borate buffer adjusted to pH 8.5, 40 mM sodium dodecyl sulfate (SDS), 12 mM beta-CD and 10% (v/v) of methanol was found to be optimal conditions for the fast separation. The contents of resibufogenin and cinobufagin were successfully determined within 5 min, with satisfactory repeatability and recovery.