HPLC法测定健脾口服液中芍药苷的含量

目的　建立健脾口服液中芍药苷含量测定方法。方法　采用HPLC法测定健脾口服液中芍药苷的含量 ,色谱柱为AlltimaC18柱 ,流动相为乙腈 水 (13∶87) ,流速为 1mL/min ,检测波长为 2 30nm ;柱温 :35℃。结果　进样量在 0 .16 5～ 6 .6 0 0 μg范围内芍药苷量与峰面积响应值呈良好的线性关系 ,r =0 .9997;平均回收率为 99.4 % ,RSD为 0 .7% (n =5 )。结论　本方法简便、准确 ,可作为该制剂的质控方法     

LC/MS analysis of brevetoxin metabolites in the Eastern oyster (Crassostrea virginica).

Brevetoxin (PbTx) metabolism was examined in the Eastern oyster (Crassostrea virginica) following exposure to a Karenia brevis red tide, by using LC/MS(/MS) and cytotoxicity assay. Metabolites observed in field-exposed oysters were confirmed in oysters exposed to K. brevis cultures in the laboratory. Previously, we identified a cysteine conjugate and its sulfoxide (MH(+): m/z 1018 and 1034) as metabolites of the brevetoxin congener PbTx-2. In the present study, we found a cysteine conjugate and its sulfoxide with A-type brevetoxin backbone structure (MH(+): m/z 990 and 1006), as probable derivatives of PbTx-1. We also found glycine-cysteine-PbTx (m/z 1047 and 1075), gamma-glutamyl-cysteine-PbTx (m/z 1147), and glutathione-PbTx (m/z 1176 and 1204) conjugates with A- and B-type backbone structures. Amino acid-PbTx conjugates react with fatty acids through amide linkage to form a series of fatty acid-amino acid-PbTx conjugates. These fatty acid conjugates are major contributors to the composite cytototoxic responses obtained in extracts of brevetoxin-contaminated oysters. Other brevetoxin derivatives found in oysters are consistent with hydrolytic ring-opening and oxidation/reduction reactions.     

通腑醒神液直肠滴注对急性脑出血意识状态的影响

目的观察通腑醒神液直肠滴注对急性脑出血神昏患者的治疗作用.方法将61例患者随机分为两组,均予西医常规处理,治疗组另予通腑醒神液直肠滴注,对照组予通腑醒神胶囊口服或鼻饲.结果两组临床疗效相近,但治疗组在促醒及减轻昏迷程度方面优于对照组.结论通腑醒神液直肠滴注是治疗急性脑出血神昏的有效方法.     

健脾消积口服液改善晚期肝癌患者生存质量32例临床研究

目的:探讨健脾消积口服液对改善晚期肝癌患者生存质量的临床疗效.方法:62例患者随机分为两组,治疗组32例与对照组30例均采用相同的西医药疗法,即保肝及对症支持疗法,治疗组32例加用健脾消积口服液治疗.结果:治疗组与对照组近期疗效总缓解率分别为62.5%和40%(P》0.05);临床证候变化比较:治疗组与对照组总改善率分别为75%和53.3%(P》0.05);生活质量变化比较:治疗组与对照组提高及稳定率分别为68.8%和43.3%;两组患者半年、1年生存率分别为65.6%、37.5%和40%、23.3%.两组比较差异有显著性(P《0.05).结论:健脾消积口服液可改善晚期肝癌患者临床症状,提高生活质量,延长生存时间;并有稳定瘤体的作用,有效地控制病情及延缓病情发展;体现了中西医结合治疗晚期肝癌的独特优势.     

Confirmation of brevetoxin metabolism in cockle, Austrovenus stutchburyi, and greenshell mussel, Perna canaliculus, associated with New Zealand neurotoxic shellfish poisoning, by controlled exposure to Karenia brevis culture.

We examined metabolism of PbTxs in New Zealand cockle, Austrovenus (A.) stutchburyi, and greenshell mussel, Perna (P.) canaliculus, by means of liquid chromatography coupled with tandem mass spectrometry. PbTx-2, PbTx-3 and BTX-B5 were detected in Karenia (K.) brevis culture medium in the ratio of ca. 50:2:5. The amounts of PbTx-3 and BTX-B5 were greatly increased in both seawater and shellfish exposed to K. brevis cultures or supernatant prepared by disruption of K. brevis under appropriate condition, while those of PbTx-2 were decreased. Some PbTx-2 was present in P. canaliculus, but not in A. stutchburyi. Low levels of BTX-B1 were detected in A. stutchburyi, but not P. canaliculus. Levels of PbTx-3 and BTX-B5 were highest immediately after exposure and then declined rapidly in both shellfish. BTX-B1 increased in concentration after exposure, and was then gradually eliminated from A. stutchburyi. Three successive exposures of A. stutchburyi to K. brevis cultures resulted in similar initial levels of PbTx-3 and BTX-B5, while BTX-B1 accumulated after each dose. In P. canaliculus, initial levels of PbTx-3 were similar, while PbTx-2 and BTX-B5 accumulated after each dose. PbTx-3 and BTX-B5 are proposed to be suitable markers for monitoring shellfish toxicity after a red tide event.     

Ambient mass spectrometry for rapid diagnosis of psychoactive drugs overdose in an unstable patient

A 25-year-old man suffered from consciousness change was sent to our emergency department by friends who reported that they were not sure what had happened to him. Physical examination revealed bilateral pupils dilatation, lethargy, slurred speech, and ataxia. Computer-aided tomographic scan of the brain revealed no definite evidence of intracranial lesions. Routine laboratory tests revealed total physiological turmoil. Despite immediate commencement of aggressive treatment, the patient's condition deteriorated long before the traditional drug screen provided an answer for the identities of the multiple drugs overdose. It ended up with the need for cardiopulmonary resuscitation, but in vain. At the end of the tragic event, under the suggestion of a colleague, a portion of the patient's urine specimen was sent to our university esoteric laboratory for rapid analysis by means of a newly-developed thermal desorption-electrospray ionization-mass spectrometry. Ketamine, 3,4-methylenedioxymethamphetamine, and 3,4-methylenedioxyamphetamine were identified in the urine sample within 30 s. Conventional toxicological testing techniques like gas chromatography–mass spectrometry or liquid chromatography-mass spectrometry are currently used for identifying abused drugs. One concern is their time-consuming sample pretreatment which leads to relatively low efficiency in terms of turnaround time for revealing the identity of the consumed drugs particularly when the patients are severely overdosed. We learned a lesson from this case that a more efficient toxicological identification technique is essential to expedite the process of emergency care when the patients are so heavily overdosed that they are under critical life-threatening conditions.     

防风通圣颗粒联合液氮冷冻治疗神经性皮炎的疗效观察

目的:评价防风通圣颗粒联合液氮冷冻治疗神经性皮炎的临床疗效和安全性。方法:120例神经性皮炎患者分为A组、B组和C组各40例,A组患者口服防风通圣颗粒,每天2次,每次3 g,液氮冷冻治疗,每周3次,连续2周为1个疗程;B组液氮冷冻治疗,每周3次,连续2周为1个疗程;C组患者口服防风通圣颗粒,每天2次,每次3 g,连续治疗2周为1疗程。结果:A组患者治疗后基愈率为75%、显效率为20%、进步率为5%、无效率为0%,有效率为95%;B组患者治疗后基愈率为55%、显效率为20%、进步率为22.5%、无效率为2.5%,有效率为75%;C组患者治疗后基愈率为52.5%、显效率为17.5%、进步率为25%、无效率为5%,有效率为70%。A组与B组、C组疗效比较差异均有显著的统计学意义(χ2=4.8039,P0.0284;χ2=7.013 0,P=0.0081);B组与C组疗效比较差异无显著的统计学意义(χ2=0.250 8,P=0.616 5)。三组患者均无明显不良反应。结论:防风通圣颗粒联合液氮冷冻治疗神经性皮炎是安全的、有效的。     

Experimental study of the influence of the counter and scintillator on the universal curves in the cross-efficiency method in LSC

The cross-efficiency method in LSC is one of the approaches proposed for the extension of the Système International de Référence (SIR) to radionuclides emitting no gamma radiation. This method is based on a so-called “universal cross-efficiency curve”, establishing a relationship between the detection efficiency of the radionuclide to be measured and the detection efficiency of a suitable tracer. This paper reports a study at LNHB on the influence of the scintillator and of the LS counter on the cross-efficiency curves. This was done by measuring the cross-efficiency curves obtained for ⁶³Ni and ⁵⁵Fe vs. ³H, using three different commercial LS counters (Guardian 1414, Tricarb 3170 and Quantulus 1220), three different liquid scintillator cocktails (Ultima Gold, Hionic Fluor and PicoFluor 15 from Perkin Elmer^®), and for chemical and colour-quenched sources. This study shows that these cross-efficiency curves are dependent on the scintillator, on the counter used and on the nature of the quenching phenomenon, and thus cannot definitively be considered as “universal”.     

3-chlorotyrosine in Sputum of COPD Patients: Relationship with Airway Inflammation

ABSTRACT

The airways of patients with chronic obstructive pulmonary disease (COPD) are associated with increased numbers of inflammatory cells, in particular neutrophils and macrophages. Contained within the primary granules of neutrophils is the heme enzyme called myeloperoxidase (MPO) that has been used as a biomarker of neutrophilic inflammation in COPD and other inflammatory diseases. MPO is the only enzyme in the body that produces hypochlorous acid (HOCl), which effectively chlorinates tyrosine residues in proteins. The presence of 3-chlorotyrosine (3Cl-Tyr) in sputum of COPD patients has yet to be established. Spontaneously produced sputum was collected from 14 stable COPD patients, and ultra-centrifuged to prepare sol phase samples for analysis. Sputum 3Cl-Tyr levels were measured using Mass Spectrometry (LC-MSMS). Sputum MPO activity was measured using a standard chromogenic substrate assay. The Spearman rank correlation was used to analyse the data. We report for the first time the measurement of 3Cl-Tyr in sputum from stable COPD patients. The sputum levels of 3Cl-Tyr correlated well with sputum MPO activity (r = 0.88; p < 0.0001). The presence of 3Cl-Tyr in the sputum of stable COPD patients suggests an active process related to MPO that may play a role in the pathophysiology of this disease.