Studies on proliferation kinetics in liver and spleen during early graft-vs-host reaction in mice.

Autoradiographic and liquid scintillation counting studies were made during the early graft-versus-host-reaction in mice. At the height of GVHR on the 10th day after transplantation, hepatosplenomegaly correlated with the radioactive disintegrations (DPM). This coincided with a high proliferation rate of the blasts that appeared in the spleen, and of the portal infiltrations and Kupffer cells in the liver. Convenient control groups were used to show that these changes are a specific reaction in GVHR.     

The sensitivity of liquid sensor,ion-selective microelectrodes to changes in temperature and solution level

Current procedures for the manufacture of ionselective microelectrodes using liquid ion sensors result in two kinds of electrode, one with a short (10–100 m) column of sensor at the tip and one with a long column (> 1 mm). We report here that the signal from a long-column microelectrode is very sensitive to small fluctuations in bath temperature and solution level when a recording is made above room temperature. This sensitivity is explained by the effects of temperature on the potentials developed at the interfaces between the ion sensor and the bordering aqueous solutions (the internal filling solution of the electrode and the test solution). If the temperature at the two interfaces is changed by different amounts, these interfacial potentials will also change by different amounts resulting in a change in the output of the electrode. Such an effect occurs for longcolumn electrodes because the column of sensor is usually not completely immersed in the heated test solution. Hence fluctuations in solution temperature and level will induce fluctuations in temperature along the column of sensor producing variations in the electrical signal from the electrode. In contrast, sensitivity to temperature and solution level is virtually absent in short-column microelectrodes since their column of sensor is fully immersed in the test solution and thereby at uniform temperature. In conclusion, in order to produce noise-free recordings of ion activities, the use of short-column microelectrodes is recommended for experiments performed above (or below) room temperature.     

Detection of five new hydroxyl analogues of azaspiracids in shellfish using multiple tandem mass spectrometry.

The polyether dinoflagellate toxins, azaspiracids, are responsible for azaspiracid poisoning (AZP), a new human toxic syndrome arising from the consumption of shellfish. To date, five azaspiracids have been isolated and fully structurally elucidated, including, AZA1, its 8-methyl and 22-demethyl analogues, AZA2 and AZA3, respectively, and two hydroxyl derivatives of AZA3, named AZA4 and AZA5. Using a recently developed method involving liquid chromatography with multiple tandem mass spectrometry (LC-MS(n)), five new azaspiracids, AZA7-AZA11, have been found in mussels (Mytilus edulis). AZA6 is a positional isomer of AZA1 and four of the new compounds are isomers with a mass of 857.5 amu. AZA7 and AZA8 are hydroxyl analogues of AZA1 while AZA9 and AZA10 are hydroxyl analogues of AZA6. AZA11 is a hydroxyl analogue of AZA2. The separation of all 11 azaspiracids was achieved using isocratic reversed phase liquid chromatography using a combination of eluent additives, trifluoroacetic acid and ammonium acetate. The ion-trap MS experiments, with electrospray ionisation, involved the fragmentation of the protonated molecule [M+H](+), trapping and fragmenting the product ions due to the loss of a water molecule [M+H-H(2)O](+), together with mass spectral data analysis that included the characteristic A-ring fragmentation for each compound.     

高效液相色谱法测定百年康口服液中橙皮苷的含量

目的：建立百年康口服液中橙皮苷的含量测定方法。方法：采用HPLC法,色谱柱为YWG C_(18)(150mm×4．6mm,5μm),流动相为乙腈-0．25%磷酸水(20∶80)；检测波长为285nm,流速为1．0mL/min。结果：橙皮苷在5～50mg/L浓度范围内呈良好的线性关系(r=0．9996),平均回收率为100．92%,RSD为1．78%。结论：本法灵敏、准确、重现性好、精密度高、专属性强,可用于百年康口服液中橙皮苷的含量测定和质量控制。     

Toxin profile of Alexandrium ostenfeldii (Dinophyceae) from the Northern Adriatic Sea revealed by liquid chromatography-mass spectrometry.

This paper reports on the first occurrence of fairly high numbers of Alexandrium ostenfeldii along the Emilia Romagna coasts (Italy). Detailed liquid chromatography-mass spectrometry (LC-MS) analyses of the toxin profile were performed on a strain of the organism collected in November 2003, isolated during the event and grown in culture. Selected ion monitoring (SIM) and multiple reaction monitoring (MRM) experiments were carried out for detection of spirolides and paralytic shellfish poisoning (PSP) toxins. They revealed that the Adriatic A. ostenfeldii produces mainly spirolide 13-desmethyl C at levels of 3.7 pg/cell but not PSP toxins. Interestingly, low levels of some spirolide isomers that have not been reported so far in other strains of the dinoflagellate were also detected. This represents the first report of spirolide-type toxins in the Adriatic Sea.     

Detection of harmful cyanobacteria and their toxins by both PCR amplification and LC-MS during a bloom event.

We briefly report here the occurrence of toxic blooms in the eutrophic reservoir Billings, S?o Paulo city, Brazil. Water samples were collected in May 2004, during a cyanobacterial bloom. The presence of toxic species was confirmed by using PCR amplifications of a fragment region of genes encoding microcystin synthetase-mcyB. The determination of toxins was performed by liquid chromatography coupled with mass spectrometry (LC-MS). LC-MS analyses of the toxins from the bloom revealed variants of microcystins (MC), such as MC-LR, MC-RR and MC-YR. HPLC-FLD was used to determine the paralytic shellfish poisoning (PSP) saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins 2 (GTX2) and 3 (GTX3). GTX2, GTX3 and NEO were detected for the first time in a natural sample from Billings reservoir. These results are a contribution to the knowledge of the biogeography of toxic cyanobacteria and their toxins, specifically in S?o Paulo.     

心舒口服液毛细管电泳指纹图谱的研究

目的对心舒口服液的质量控制方法进行研究。方法采用高效毛细管电泳法建立以10批当归道地药材,10批川芎道地药材,10批红花道地药材,10批心舒口服液为样品的指纹图谱,比较研究制剂与药材指纹图谱之间的相关性,并与单味药材水煎液、各药材阴性对照液的指纹图谱进行比较,通过比较在线紫外光谱和迁移时间的方法,对口服液与各药材的水煎液、阴性对照液的指纹图谱中各指纹峰进行一一归属。结果分别建立标准指纹图谱,初步确定样品制剂与原料药材指纹图谱之间的相关性,最终建立复方中药制剂的质量控制方法。结论在心舒口服液指纹谱中,27个指纹峰中有14个指纹峰来自当归,10个指纹峰来自川芎(其中7个指纹峰是当归与川芎所共有的),9个指纹峰来自红花。     

液相色谱-质谱/质谱联用技术分析18种游离氨基酸

目的：建立氨基酸的液相色谱-质谱检测方法。方法：无需衍生处理，直接用乙腈：水：甲酸（5：95：0．1．v／v／v）为流动相进行反相液相色谱分离，用电喷雾正离子源进行离子化，选择反应监测方式（SRM）对这18种氨基酸的母离子及子离子进行监测，三级四极质谱测定。结果：该方法抗干扰能力强，方法重现性好，RSD0．4％。3．7％，回收率95％～104％，相关系数0．9931-0．9999，检出限0．5～8mol／ml。结论：该方法简单、快速、准确、灵敏，适合测定各种样品中的游离氨基酸。     

健胃口服液抗消化性溃疡的药理研究

目的：探讨健胃口服液抗消化性溃疡的药理作用。方法：采用水浸应激、幽门结扎、利血平诱发及乙酸损伤等方法造成急慢性胃溃疡模型,观察药物对这些模型的影响。结果：健胃口服液对大白鼠急性应激性溃疡、幽门结扎型溃疡、乙酸损伤型溃疡、小白鼠利血平诱发型溃疡的形成均具有显著的抑制作用（P＜0．05,P＜0．01）,能显著减少胃酸及胃蛋白酶的分泌（P＜0．05）。结论：健胃口服液具有防治消化性溃疡的作用。     

金龙蛇口服液合参麦注射液对中晚期胃癌患者肿瘤标志物和免疫功能的影响

应用中药金龙蛇口服液及参麦注射液治疗中晚期胃癌患者35例,并与应用化疗的16例患者对照,结果应用中药治疗的患者,体力指数（Karnofsky评分）及NK细胞活性明显升高,CD4,CD4／CD8亦明显升高,CD8明显下降,与治疗前比较差异均有显著性（P＜0．05）,而化疗组除CD4／CD8略有改善外,NK细胞活性,CD3,CD4较治疗前下降,两组肿瘤标志物CEA及CA19－9也有一定程度下降,但与治疗前比较无明显差异（P＞0．05）,提示中药金龙蛇口服液及参麦注射液联合应用治疗中晚期胃癌有良好作用。