HPLC法测定注射用阿奇霉素的含量

目的：建立反相高效液相法测定注射用阿奇霉素含量的方法。方法采用Inertsil ODS柱（4．6 mm ×250 mm,5μm）,以0．1 mol·L－1乙酸铵（用氨水调节pH值至8．6）—乙腈—甲醇（50∶30∶20）为流动相,流速1．0 mL·min－1,检测波长218 nm,柱温60℃。结果阿奇霉素的线性范围为100～2000 mg·L－1,r＝0．9998,平均回收率98．8％,RSD＝0．6％（n＝9）。结论该方法简便快速、准确,更适于控制注射用阿奇霉素的质量。     

高效液相色谱法测定人血浆中苯巴比妥浓度

目的：建立测定人血浆中苯巴比妥浓度的高效液相色谱法。方法以 DiamonsilTM C18反相柱（150mm ×4．6mm，5μm）为色谱柱，流动相为50mmol? L－1醋酸铵－甲醇（15∶85 V／V）；流速：1．0mL? min －1；检测温度：30℃；检测波长：230nm。提取剂为乙酸乙酯与二氯甲烷（90∶10 V／V）。结果苯巴比妥的低、中、高（4．0，16．0，48．0μg? mL－1）3个浓度点平均相对回收率均大于95％，提取回收率大于75％；日内、日间相对标准偏差（RSD）均低于15％（n＝5）；分析方法的检测限1．0μg? mL －1；苯巴比妥在2．0～64．0μg? mL －1范围内线性关系良好，r＝0．9998（n ＝7）。线性方程：Y＝3．182X＋1．06。结论该方法灵敏、准确、简单、快速，可用于苯巴比妥临床血药浓度监测和药动学研究。     

HPLC法测定磷酸伯氨喹片溶出度

目的：采用高效液相色谱法（HPLC）测定磷酸伯氨喹片剂溶出度,并进行方法科学性考察。方法采用浆法,以0．01mol? L －1盐酸溶液900mL为溶出介质,转速50r? min －1,溶出时间为60min。采用 HPLC法检测,色谱柱为辛烷基硅烷键合硅胶柱（Inertsil,4．6mm ×75mm,3μm）,流动相为水－乙腈－四氢呋喃－三氟乙酸（90∶9∶1∶0．1,V／V／V／V）,流速为1．5mL? min －1,进样量50μL,于265nm处测定色谱图。结果磷酸伯氨喹浓度在7．019～21．058μg? mL －1范围内线性关系良好r＝0．9999（n＝5）,精密度良好（RSD ＝0．26％,n＝6）,平均回收率为100．2％（RSD ＝0．5％）,溶液在24h以内有较好的稳定性（RSD＝0．3％）,定量限为0．1μg? mL －1,在60min时的主成分溶出率可达到溶出平衡点。结论该法具有准确、可靠、稳定的优点,适用于磷酸伯氨喹片剂溶出度的测定。     

HPLC法测定小建中颗粒中芍药苷和肉桂酸的含量

目的：采用高效液相色谱法测定小建中颗粒中芍药苷和肉桂酸的含量。方法采用Ultimate XB－C18（4．6×250mm,5μm）色谱柱;乙腈－水（17∶83）为流动相;流速1．0mL? min －1;检测波长230nm,柱温：30℃。结果芍药苷和肉桂酸在20－200μg? mL －1（r＝0．9999）,0．2～20μg?mL －1（ r＝0．9997）范围内线性关系良好,平均加样回收率为101．58％、99．52％, RSD 分别为2．43％（ n ＝6）和2．23％（ n ＝6）。结论本法简便、准确,可作为该制剂的质量控制方法。     

HPLC法测定胆仙胶囊中绿原酸的含量

目的：建立测定胆仙胶囊中绿原酸含量的方法。方法采用高效液相色谱法。色谱柱为依利特C18（4．6mm ×250mm,5μm）,流动相为乙腈－0．1％磷酸水溶液（20∶80,V／V）,流速为1．0mL? min －1,检测波长为327nm,进样量为10μL。结果绿原酸的质量浓度线性范围为14．0～140μg? mL－1（r＝0．9992,n＝6）;平均加样回收率为99．52％,RSD为0．73％（n＝9）。结论本方法快速、简便、准确、重现性良好,可用于该制剂的质量控制。     

HPLC法测定卡泊三醇倍他米松凝胶的含量

目的：建立了HPLC测定卡泊三醇倍他米松凝胶倍他米松的含量。方法色谱柱为 C18柱（4．6mm ×250mm,5μm）,流动相为甲醇－水（70∶30）,流速为1．0mL? min －1,检测波长为240nm。结果倍他米松的线性范围为30～100μg? mL －1（r ＝1．000）,平均回收率为99．3％, RSD为0．5％。结论该方法简便、准确、快速,重复性好。     

高效液相色谱测定比格犬血浆中的头孢唑啉与头孢曲松的浓度

目的：建立HPLC在多项测定参数相同的基础上,分别测定比格犬血浆中头孢唑啉、头孢曲松浓度的方法。方法色谱柱：头孢唑啉为ES industries Epic C18（4．6 mm ×150 mm,5μm）,头孢曲松为Phenomenex Gemini C18（4．6 mm ×150 mm,5μm ）,流动相：头孢唑啉为甲醇－0．05 mol? L－1乙酸铵缓冲液（ pH＝4．3）＝30∶70;头孢曲松为乙腈－0．05 mol? L－1 KH2 PO4缓冲液（ pH＝6．0）＝6∶94,流速均为1．0 mL? min－1,进样量均为40μL。结果头孢唑啉标准曲线回归方程为 y ＝－1．25×104 x ＋8479．37（ r ＝0．9974）,头孢曲松为y＝1．25×104 x ＋2．72×104（ r ＝0．9976）。头孢唑啉线性范围为2～300μg? mL－1,头孢曲松为2～200μg? mL－1;日内、日间精密度相对标准偏差均≤10％,提取回收率均≥85．78％。结论本法灵敏、准确、快速,可用于比格犬血浆头孢唑啉、头孢曲松浓度的测定和药物其他方面研究。     

高效液相色谱法测定阿奇霉素片的含量

目的用高效液相色谱（HPLC）法测定阿奇霉素片的含量。方法采用Phenomenex C18（250mm×4．6mm,5μm），流动相为0．067mol／L的磷酸二氢铵溶液（用三乙胺调pH值至6．5）-乙腈（65：35），流速为1mL／min，检测波长为205nm。结果阿奇霉素质量浓度在1.01-3.02mg／mL范围内与峰面积线性关系良好，r=0.9993，平均回收率为99.2％，RSD=0.93％（n=5）。结论HPLC法测阿奇霉素片含量准确可靠，重现性好。     

HPLC法测定消渴丸中葛根素的含量

目的：建立HPLC法测定消渴丸中葛根素含量的方法。方法采用Scienhome C18（250mm ×4．6mm，5μm）色谱柱，以甲醇－水（25∶75）为流动相，流速为1．0mL? min －1，检测波长为250nm。结果葛根素的线性范围为82．4～824ng（r＝0．9999），平均回收率为99．84％，RSD 为0．5％（n＝5）。结论该方法结果准确，灵敏度高，重复性好，可用于消渴丸的质量控制。     

HPLC法同时测定颈舒颗粒中天麻素和桂皮醛的含量

目的：建立HPLC法同时测定颈舒颗粒中天麻素和桂皮醛含量测定的方法。方法采用高效液相色谱法,色谱柱：Platisil ODS 柱（4．6mm ×250mm,5μm）,流动相：乙腈（A）－水（B）;梯度洗脱;流速1．0mL? min －1;柱温30℃;检测波长：天麻素为220nm,桂皮醛为290nm;进样量：10μL。结果天麻素和桂皮醛分别在在10．32～206．40μg? mL －1（r ＝0．9998,n＝6）、8．97～179．40μg? mL －1（r ＝0．9999,n＝6）范围内与其峰面积呈良好的线性关系。天麻素和桂皮醛的平均加样回收率分别为为100．79％、99．10％,RSD分别为1．32％、1．36％（ n＝6）。结论该方法操作准确、简便、重现性好,可用于颈舒颗粒中天麻素和桂皮醛的含量测定。     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.