Determination of chlorate and perchlorate in eggs by ultra performance liquid chromatography-tandem mass spectrometry / 国际药学研究杂志

Objective: To establish a method for the determination of chlorate and perchlorate in eggs by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods: After homogenizing, the egg samples were extracted with 0.1% formate water-acetonitrile,purified by PRIME HLB column,and separated by Thermo Acclaim™ Trinity™ P1 ion exchange column. Eluates from the HPLC system were introduced into Waters Xevo TQ-XS triple quadrupole UPLC-MS/MS system in negative electrospray ionization mode using multiple reaction monitor- ing(MRM),with chlorate18O3 and perchlorate18O4 as internal standard. Results: The chlorate had a good linear rela- tionship in the range of 0.2-100.0 μg/L,with R>0.999. Perchlorate had a good linear relationship in the range of 0.1-50.0 μg/L,with R>0.999. The average recovery of chlorate was 95.7-109.4%,and the precision was 3.0-9.1%. The average recovery of perchlorate was 95.6%-115.3%,and the precision was 2.1%-8.6%. Conclusion: The estab- lished method appears to be simple,rapid,accurate,sensitive,and suitable for the determination of chlorate and per- chlorate in high protein samples.

Neutrophil-mimicking therapeutic nanoparticles for targeted chemotherapy of pancreatic carcinoma

Due to the critical correlation between inflammation and carcinogenesis, a therapeutic candidate with anti-inflammatory activity may find application in cancer therapy. Here, we report the therapeutic efficacy of celastrol as a promising candidate compound for treatment of pancreatic carcinoma naïve neutrophil membrane-coated poly(ethylene glycol) methyl ether--poly(lactic--glycolic acid) (PEG-PLGA) nanoparticles. Neutrophil membrane-coated nanoparticles (NNPs) are well demonstrated to overcome the blood pancreas barrier to achieve pancreas-specific drug delivery . Using tumor-bearing mice xenograft model, NNPs showed selective accumulations at the tumor site following systemic administration as compared to nanoparticles without neutrophil membrane coating. In both orthotopic and ectopic tumor models, celastrol-loaded NNPs demonstrated greatly enhanced tumor inhibition which significantly prolonged the survival of tumor bearing mice and minimizing liver metastases. Overall, these results suggest that celastrol-loaded NNPs represent a viable and effective treatment option for pancreatic carcinoma.

Synthesis, characterization and theoretical calculations of Cu(I) complex of trithiocyanuric acid [Cu(ttc)3] / Síntesis, caracterización y cálculos teóricos del complejo Cu(I) de ácido cianúrico [Cu(ttc)3] / Síntese, caracterização e cálculos teóricos do complexo Cu(I) de ácido cianúrico [Cu(ttc)3]

Abstract A new Cu(I) complex constructed by reaction of trithiocyanuric acid (ttc) and copper(II) perchlorate hexahydrate has been successfully synthesized by a slow sedimentation method in a DMF solvent at room temperature. The molecular structure of the compound was elucidated by MALDI-TOF MS, UV-Vis and FTIR spectroscopy, DSC-TGA analysis and magnetic susceptibility measurement. The proposed structure was corroborated by a computational study carried out with the Gaussian09® and AIMAII® programs using the RB3LYP hybrid DFT functional with both 6-31G and Alhrich-TZV basis sets. The calculated vibrational frequencies values were compared with experimental FTIR values. Photophysical properties of the synthesized complex were evaluated by UV-Visible spectroscopy and compared with computed vertical excitation obtained from TDDFT. The theoretical vibrational frequencies and the UV-Vis spectra are in good agreement with the experimental values. Additionally, the Frontier Molecular Orbitals (HOMO - LUMO) and the Molecular Electrostatic Potential of the complex was calculated using same theoretical approximation. The results showed the interaction between three coordinated ligand atoms and the Cu(I) ion.

Resumen Un nuevo complejo de Cu(I) elaborado por la reacción de ácido cianúrico (ttc) y perclorato de cobre(II) hexahidrato se sintetizó exitosamente por medio de un método lento de sedimentación en un solvente de DMF a temperatura ambiente. La estructura molecular del compuesto se determinó utilizando MS de MALDI-TOF, la espectroscopia de UV-VIS y de FTIR, el análisis de DSC-TGA y el análisis magnético de susceptibilidad. La estructura propuesta se corroboró por medio de un estudio computacional usando los programas Gaussian09® y AIMAII®, utilizando el híbrido RB3LYP DFT con los equipos 6-31G y Alhrich-TZV. Se compararon los valores calculados de las frecuencias vibracionales con los valores experimentales de FTIR. Se evaluaron las características fotofísicas del complejo sintetizado usando espectroscopia UV-visible y se compararon con la vibración vertical obtenida de TDDFT. Las frecuencias teóricas vibracionales y los espectros UV-VIS coinciden con los valores experimentales. Además, se calcularon las órbitas moleculares (HOMO - LUMO) y el potencial electrostático molecular del complejo usando la misma aproximación teórica. Los resultados demostraron la interacción entre tres receptores de átomos coordinados y el ion del Cu(I).

Resumo Um novo complexo de Cu(I) elaborado pela reação de ácido cianúrico (ttc) e perclorato de cobre (II) hexahidratado foi sintetizado de maneira exitosa por meio de um método lento de sedimentação em um solvente de DMF a temperatura ambiente. A estrutura molecular do composto se determinou utilizando MALDI-TOF, espectroscopia de UV-VIS e FTIR, DSC-TGA e análise magnético de susceptibilidade. A estrutura proposta se corroborou por meio de um estudo computacional usando os programas Gaussian09® e AIMAII®, utilizando o híbrido RB3LYP DFT com os equipamentos 6-31G e Alhirich-TZV. Se compararam os valores calculados das frequências vibracionais com os valores experimentais de FTIR. Se avaliaram as características fotofísicas do complexo sintetizado utilizando espectroscopia UV-VIS e se compararam com a vibração vertical obtida de TDDFT. As frequências teóricas vibracionais e os espectros UV-VIS coincidem com os valores experimentais. Além disso, se calcularam as órbitas moleculares (HOMO - LUMO) e o potencial eletrostático molecular do complexo utilizando a mesma aproximação teórica. Os resultados demonstraram a interação entre três receptores de átomos coordenados e o íon de Cu(I).

Alteraciones leucocitarias por exposición a perclorato de amonio en ratones de la cepa ICR / Leucocitary changes by ammonium perchlorate in ICR mice strain / Alterações leucocitárias por exposição a perclorato de amônio em camundongos da linhagem ICR

El presente trabajo tuvo como objetivo identificar alteraciones en el recuento de leucocitos en sangre periférica, generadas por la exposición a perclorato de amonio, en ratones de la cepa ICR, evaluando diferentes concentraciones de exposición y diferenciando dichas alteraciones en machos y hembras. Se realizó mediante un trabajo de diseño analítico tipo experimental. Se utilizaron 60 ratones de la cepa ICR, 30 machos y 30 hembras de los cuales 50 fueron expuestos a perclorato de amonio. La manipulación se llevó a cabo de acuerdo con lo establecido en la resolución 008430 de 1993, artículo 87 del Ministerio de Salud de la República de Colombia. Un 70% de los ratones hembra y un 83% de los ratones macho expuestos a perclorato de amonio presentaron alteraciones en el recuento celular de la línea blanca. Los machos presentaron mayor alteración leucocitaria, en especial linfocitopenia. Por otro lado, el peso en los ratones expuestos disminuyó considerablemente hacia la tercera semana de administración de perclorato de amonio, lo cual podría indicar que esta sustancia tóxica genera un estado de inmunosupresión. Se evidenció leucopenia, específicamente neutropenia, neutrofilia y linfocitopenia como principales alteraciones en el recuento de leucocitos en ratones de la cepa ICR, expuestos a perclorato de amonio.

The objective of this work was to identify the changes in the leukocyte counts in peripheral blood by ammonium perchlorate in ICR strain mice, evaluating the different exposure concentrations and differentiating the changes between males and females. Through an analytic experimental investigation, 60 ICR strain mice, 30 males and 30 females were used, 50 of which were exposed to ammonium perchlorate. This study was carried out by Resolution 008430/93, article 87 of Ministry of Health of Colombia. A total of 70% females and 83% males had changes in the leukocyte counts, especially lymphocytopenia in males, further, weight decreased the third week of treatment, and probably that toxic substance induces a state of immunosuppression. The main changes in the leukocyte counts in peripheral blood by ammonium perchlorate in ICR strain was leukopenia.

O objetivo deste trabalho foi identificar as alterações na contagem de leucócitos em sangue periférico, geradas pela exposição a perclorato de amônio em camundongos da linhagem ICR, avaliando diferentes concentrações de exposição e diferenciando estas alterações entre machos e fêmeas. Isto foi realizado através de um trabalho de desenho analítico tipo experimental. Foram utilizados 60 camundongos da linhagem ICR, sendo 30 machos e 30 fêmeas, dos quais 50 foram expostos ao perclorato de amônio. O manuseio foi realizado conforme a resolução 008430 de 1993, artigo 87 do Ministério da Saúde da Colômbia. 70% dos camundongos fêmea e 83% dos machos apresentaram alterações na contagem celular dos leucócitos, especialmente a linfocitopenia em machos. Além disso, o peso nos camundongos expostos diminuiu en forma considerável para a terceira semana de tratamento com perclorato de amônio, o qual poderia indicar que esta substância tóxica gera um estado de imunossupressão. Houve evidência de leucopenia, especificamente neutropenia, neutrofilia e linfocitopenia como principais alterações na contagem de leucócitos em camundongos da linhagem ICR, expostos a perclorato de amônio.

Perchlorate contamination exposure assessment on commercial foods in Shanghai / 上海预防医学

Objective To ascertain the perchlorate contamination level in commercial foods and health risks so as to provide reference for perchlorate standard formulation and risk management.Methods Perchlorate risk survey was done on commercial foods in Shanghai;in combination with the survey results of residents'' food consumption,the exposure assessment on the presence of perchlorate in commercial food was performed by probability assessment approach.Results A total of 80 food samples from 8 food categories were analyzed,including grain,vegetables,fruits,dairy products,meat,eggs,aquatic products and teaand perchlorate detection rate was 78.8% with a mean value as 13.0±26.4 μg/kg.The highest mean value of perchlorates was 59.0±51.9 μg/kg in tea,and the lowest mean value was 3.4±2.3 μg/kg in fruits.With protection of human life and health as the maximum principle (there were supposed to be no losses of perchlorate during food processing),it was found that the estimated average dietary intake of perchlorate from the 8 food categories was 0.25 μg/kgbw.However,the 95 percentile exposure estimates reached up to 0.44 μg/kgbw,which exceeded the tolerable daily intake value of 0.3μg/kgbw established by European Food Safety Authority for healthy adults.Therefore,potential health risk may exist to certain groups of people.Conclusion Due to its high water-solubility,degradation of perchlorate in food processing probably occurs to certain extent.Therefore,there is need to carry out further actual exposure study.

Determination of perchlorate in food by ultra performance liquid chromatography-tandem mass spectrometry / 中国食品卫生杂志

Objective To establish a method for the determination of perchlorate in food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Methods The perchlorate residue in spices and condiments was extracted with water,that in vegetables and fruits was extracted with acetonitrile-water (1∶ 1,V/V),and that in meat,poultry,eggs,milk and aquatic products was extracted with acetonitrile-water (2∶ 1,V/V).The supernatant was cleaned up with C18 SPE (3 ml,200 mg),and the detection was carried out by UPLC-MS/MS with internal standardmethod for quantification.Results The calibration curve was linear in the concentration range of 0.3-20.0 pg/L (R2 ≥0.999),the recovery was in the range of 82.6％-108.6％,the relative standard deviation (RSD) was in the range of 1.0％-9.9％,and the limit of detection was 2.0 μg/kg for milk,and 10.0 μg/kg for other food.Conclusion The method was simple,accurate and highly sensitive,and suitable for the determination of perchlorate in food.

Role of vagus nerve on Diethylnitrosamine-induced hepatocellular carcinoma in rats / 中华肝胆外科杂志

Objective To study the role of vagusism on diethytlnitrosamine (DEN)-induced hepatocellular carcinoma in rats and to explore its mechanism.Methods The rat vagus nerve was labeled with 1,1'-dioctadecyl-3,3,33 -tetramethylindocarbocyanine perchlorate (DiI) tracer.The rats were divided into three groups:cancer induced rat models (cancer-induced group,n =20),cancer-induced and vagal detachment models (combined group,n =20) and normal rats (negative group,n =20),HE staining was performed on the liver tissue biopsied from the three groups of rats.The pathological grading score was evaluated and statistically analyzed.Immunohistochemistry (IHC) staing was used to determine the expression of vagal neurotransmitters and related receptors in liver tissue.Results The optimal concentration (1 mg/ml) and fixation duration with formalin (4 days) of DiI tracer marker vagal nerve demonstrated superior distribution and density of vagus nerve in the liver tissue.The incidence of hepatocellular carcinoma was significantly higher in the cancer-induced group (75％) than combined group (15％),the difference was statistically significant (P ＜ 0.05).IHC staining results of acetllcholine showed a significant difference between cancerinduced group (9.10) and combined group (2.30) or negative group (2.95),the difference was statistically significant (P ＜ 0.05).The M1 receptor expression was significantly higher in cancer-induced group (6.00) than combined group (2.30) and negative group (2.55),the differences were statistically significant (P ＜ 0.05).There was no significant difference of M2 receptor expression among the cancer-induced group (1.30),combined group (1.25) and negative group (1.35) (P ＞ 0.05).The M3 receptor expression detected with IHC staining shown there were statistical differences among cancer-induced group (8.95),combined group (6.30) and negative group (3.60) (all P ＜ 0.05).Conclusion The vagus nerve may play an important role in the development of DEN-induced hepatocellular carcinoma in rats.

Propylthiouracil, Perchlorate, and Thyroid-Stimulating Hormone Modulate High Concentrations of Iodide Instigated Mitochondrial Superoxide Production in the Thyroids of Metallothionein I/II Knockout Mice

BACKGROUND: Increased oxidative stress has been suggested as one of the underlying mechanisms in iodide excess-induced thyroid disease. Metallothioneins (MTs) are regarded as scavengers of reactive oxygen species (ROS) in oxidative stress. Our aim is to investigate the effects of propylthiouracil (PTU), a thyroid peroxidase inhibitor, perchlorate (KClO4), a competitive inhibitor of iodide transport, and thyroid stimulating hormone (TSH) on mitochondrial superoxide production instigated by high concentrations of iodide in the thyroids of MT-I/II knockout (MT-I/II KO) mice. METHODS: Eight-week-old 129S7/SvEvBrd-Mt1(tm1Bri) Mt2(tm1Bri)/J (MT-I/II KO) mice and background-matched wild type (WT) mice were used. RESULTS: By using a mitochondrial superoxide indicator (MitoSOX Red), lactate dehydrogenase (LDH) release, and methyl thiazolyl tetrazolium (MTT) assay, we demonstrated that the decreased relative viability and increased LDH release and mitochondrial superoxide production induced by potassium iodide (100 µM) can be relieved by 300 µM PTU, 30 µM KClO4, or 10 U/L TSH in the thyroid cell suspensions of both MT-I/II KO and WT mice (P<0.05). Compared to the WT mice, a significant decrease in the relative viability along with a significant increase in LDH release and mitochondrial superoxide production were detected in MT-I/II KO mice(P<0.05). CONCLUSION: We concluded that PTU, KClO4, or TSH relieved the mitochondrial oxidative stress induced by high concentrations of iodide in the thyroids of both MT-I/II KO and WT mice. MT-I/II showed antioxidant effects against high concentrations of iodide-induced mitochondrial superoxide production in the thyroid.

Test of chemical dyes and quantitative determination of dracorhodin perchlorate in Guanmaining tablets / 中国药学杂志

OBJECTIVE: To establish methods for the test of chemical dyes and quantitative determination of dracorhodin perchlorate in Guanmaining tablets. METHODS: HPLC-UV-MS/MS was used for the test of chemical dyes in Guanmaining tablets, and the concentration of dracorhodin perchlorate was determined by HPLC. In the test of chemical dyes, Agilent Zorbax-SB C18 (4.6 mm × 250 mm, 5 μm) was used as stationary phase, the mixture of 0.02 mol · L-1 ammonium acetate and acetonitrile was used as mobile phase in gradient elution mode, and the UV-Vis detection wavelength was set at 520 nm. ESI+ was used as ion source, and the MS/MS spectra of the analytes were recorded to confirm the positive results. In the quantitative analysis of dracorhodin perchlorate, Phenomenex Luna C18(4.6 mm × 250 mm, 5 μm) was used as stationary phase, the mixture of acetonitrile and 0.05 mol · L-1 sodium dihydrogen phosphate solution (37:63) was used as mobile phase, and the detection wavelength was set at 440 nm. RESULTS: Among 56 batches of Guanmaining tablets, 7 batches showed positive results of sudan I, sudan IV, and/or 808 scarlet. A good linear relationship was obtained in the range of 0.408 0 - 816.6 μg · mL-1 for dracorhodin perchlorate, with the linear regression equation of y = 1.746 1 × 107ρ +2 419.9(r = 1.000 0); the average recovery was 98.37% (RSD = 1.2%, n =6). The content of dracorhodin perchlorate in Guanmaining tablets ranged from 0.01 to 0.25 mg · tablet-1. CONCLUSION: The method is simple, accurate and rapid, and can be used for the quality control of Guanmaining tablets.

Análisis de la relación entre alteraciones del eje hipotálamo-hipófisis-tiroides y exposición a perclorato en ratones de la cepa ICR / Analysis of alterations between the hypothalamic-pituitary-thyroid axis and perchlorate exposure in ICR mice strain

Este estudio establece una correlación entre la exposición a perclorato de amonio y la presencia clínica de alteraciones en el eje hipotálamo-hipófisis- tiroides, tomando como referencia diferentes dosis de aplicación desde la aceptada como dosis segura hasta un incremento significativo de dicha dosis. El trabajo reviste gran importancia debido a que esta sustancia química es uno de los compuestos de mayor uso como pesticida en el departamento de Boyacá. Mediante ensayos inmunoenzimáticos con microplacas; con los Kit comerciales Kit Accubind Elisa Microwells TSH y Kit Accubind Elisa Microwells T4L y el análisis clínico se pudo establecer la existencia de alteraciones en el eje hormonal, lo que puede ser indicador en el futuro de un alto riesgo por parte de los individuos que manipulen esta sustancia.

This study establishes a correlation between exposure and clinical alterations in the hypothalamic-pituitary-thyroid axis. Different dosages were applied, from the accepted safe dosage up to a significant increase dosage. The study was carried out under the laboratory animal center conditions at Universidad of Boyacá (Colombia). Due that ammonium perchlorate is one of the most used compounds as pesticide in Boyacá department this type of studies are extremely important. Using enzyme immunoassay in micro-plate (Accubind Elisa Microwells TSH and Kit Accubind Elisa Microwells T4L ) and following clinical analysis alterations in the hormonal axis were found which could be be indicative of a possible high risk in the future for individuals who handle this substance.

Dracorhodin Perchlorate Suppresses Proliferation and Induces Apoptosis in Human Prostate Cancer Cell Line PC-3 / 华中科技大学学报（医学）（英德文版）

The growth inhibition and pro-apoptosis effects of dracorhodin perchlorate on human prostate cancer PC-3 cell line were examined.After administration of 10-80 μmol/L dracorhodin perchlorate for 12-48 h,cell viability of PC-3 cells was measured by MTT colorimetry.Cell proliferation ability was detected by colony formation assay.Cellular apoptosis was inspected by acridine orange-ethidium bromide fluorescent staining,Hoechst 33258 fluorescent staining,and flow cytometry (FCM) with annexin V-FITC/propidium iodide dual staining.The results showed that dracorhodin perchlorate inhibited the growth of PC-3 in a dose- and time-dependent manner.IC50 of dracorhodin perchlorate on PC-3 cells at 24 h was 40.18 μmol/L.Cell clone formation rate was decreased by 86％ after treatment with 20 μmol/L of dracorhodin perchlorate.Some cells presented the characteristic apoptotic changes.The cellular apoptotic rates induced by 10-40 μmol/L dracorhodin perchlorate for 24 h were 8.43％ to 47.71％ respectively.It was concluded that dracorhodin perchlorate significantly inhibited the growth of PC-3 cells by suppressing proliferation and inducing apoptosis of the cells.

Analysis and Exposure Assessment of Perchlorate in Korean Dairy Products with LC-MS/MS

OBJECTIVES: Perchlorate is an emerging contaminant that is found everywhere, including various foods. Perchlorate is known to disturb the production of thyroid hormones and leads to mental disorders in fetuses and infants, as well as metabolic problems in adults. In this study, we attempted to establish an LC-MS/MS method for measuring perchlorate in dairy products and used this developed method to investigate perchlorate levels in Korean milk and yogurt samples. METHODS: The developed method of perchlorate analysis requires a shaker and 1% acetic acid/acetonitrile as the extracting solvent. Briefly, the samples were extracted and then centrifuged (4000 rpm, 1hour), and the supernatant was then passed through a Envitrade mark Carb SPE cartridge that had been prewashed sequentially with 6 mL of acetonitrile and 6 mL of 1% acetic acid in water. The final volume of the sample extract was adjusted to 40 mL with reagent water and the final sample was filtered through a 0.20-microm pore size PTFE (Polytetrafluoroethylene) syringe filter prior to LC-MS/MS. RESULTS: The average levels of perchlorate in milk and yogurt samples were 5.63 +/- 3.49 microg/L and 3.65 +/- 2.42 microg/L, respectively. The perchlorate levels observed in milk samples in this study were similar to those reported from China, Japan, and the United States. CONCLUSIONS: The exposure of Koreans to perchlorate through the consumption of dairy products was calculated based on the results of this study. For all age groups, the calculated exposure to perchlorate was below the reference of dose (0.7 microg/kg-day) proposed by the National Academy of Science, USA, but the perchlorate exposure of children was higher than that of adults. Therefore, further investigation of perchlorate in other food samples is needed to enable a more exact assessment of exposure of children to perchlorate.

Zinc perchlorate-alumina: A mild, efficient catalyst for ring opening of epoxides with amines: An improved protocol for the synthesis of Β-amino alcohols.

The epoxides undergo smoothly ring-opening reaction with various amines catalyzed by zinc perchlorate on alumina under mild reaction conditions. All the reactions were carried out at room temperature to afford the corresponding b-amino alcohols in excellent yields. The catalyst was recovered and reused further reactions with very good efficiency.

Magnesium perchlorate [Mg (ClO4)2] catalyst one-pot synthesis of 3,4-DI hydropyrimidin-2(1H)-ones: an improved procedure for biginelli condensation.

3, 4-Dihydropyrimidinones were synthesized very efficiently in excellent yields, while using the magnesium perchlorate as catalyst. This protocol can be applicable to a wide range of aldehydes, ethylacetoacetate and urea. The reaction conditions were very mild and the isolation of products also very easy.

Research Advance in Effect of Perchlorate on Human Health / 环境与健康杂志

Perchlorate is a new emerging environmental pollutant that is very stable and persistent,and it can diffuse rapidly in the environment. The environmental problems caused by perchlorate have attracted a great attention from many environmental scientists. However,up to now,a few reports on perchlorate pollution have been reported in China. In this paper,for perchlorate as an environmental pollutant,the sources,characteristics,detecting methods and toxicological effect on human body were reviewed,and the further research topics were presented.

The effects of ammonium perchlorate (AP) on pulmonary fibrosis / 中华急诊医学杂志

Objective To explore the effects of AP on pulmonary fibrosis. Methods Alveolar macrophages (AM) were treated by AP for 24 hours. Pulmonary fibroblasts (FB) were cultured with the supernatant of AM medium. The protein of transforming growth factor beta 1 (TGF-?1) of AM, the proliferative activity and hydroxyproline (Hyp) content of FB were examined. Rats were treated with AP by intratracheal instillation and sacrificed at 3 days. The TGF-?1 mRNA content in the lung was examined. Results The positive staining macrophages in low and high AP groups and the quantity of TGF-?1 in high AP group were obviously higher than those in the control group (P

Preparation and Quality Control of Powder of Promoting Blood Circulation to Arrest Pain / 中国药房

OBJECTIVE:To prepare powder of promoting blood circulation to arrest pain and to establish its quality con?trol method.METHODS:Qualitative identification of panax pseudo-ginseng,frankincense and dragon blood in the powder of promoting blood circulation to arrest pain was performed by TLC method.The content of dracorhodin in the dragon blood was determined by TLC Scanning Method.RESULTS:Good linear relationship was achieved when the sample size of dracorhodin perchlorate remained within the scope of0.6?g～3.2?g(r=0.9999).The average recovery rate was98.22%(RSD=1.53%).CONCLUSION:This preparation method is feasible,and the quality control method is simple,accurate and reproducible.

Perchlorate discharge test.

A variety of perchlorate discharge techniques was performed and the criteria for interpretation varied according to the techniques employed. The modified technique, 10 microcurrie of Na131 I was injected into the patient with a 10 minute serial recording for 1 hour ; KC 104 300 mg/25 ml was given orally and continued with 10 minute serial recording for 30 minutes. This technique can identify the iodide transport defect and organic binding defect of the thyroid gland, and trapping function of the gland. In 25 mormal subjects, the thyroid131 I- content increased during a 60 minute serial recording and after KC 104 was given. The discharge observed during 90 minutes ranged from 1% to (- 55.7%). The range at the 20 – minute uptake is from 4.70% to 11.66% (X ฑ 2 SD). In 15 patients, 3 patients had iodide transport defect, 9 patients organic binding detect, while such defects could not be found for the remaining patients. However, it is possible that the remaining three may have other kinds of defects such as iodotyrosine coupling defect, iodotyrosine dehalogenase defect or abnormal secretion of iodoprotein.