HPLC法测定磷酸川芎嗪葡萄糖注射液的含量及有关物质

目的:建立磷酸川芎嗪葡萄糖注射液含量及葡萄糖降解产物5-羟甲基糠醛(5-HMF)的测定方法。方法:采用高效液相色谱法,色谱柱为Inertsil C_(18)(5μm,4.6 mm×150 mm),流动相为甲醇-水-磷酸(25:75:0.13),流速0.8 mL·min~(-1),UV295 nm检测。结果:川芎嗪在0.12-0.92 mg·m~(-1)范围内r=0.9997(n=5);5-HMF在0.14-11.4μg·mL~(-1)范围内r=0.9999(n=11),线性关系良好。川芎嗪和5-HMF的检测限分别为0.8 ng和0.5 ng。分析了3批样品,川芎嗪的含量为标示量的99.4%-100.0%。主要有关物质5-HMF为0.29-0.35μg·mL~(-1),未见其他有关杂质。结论:该法同时测定川芎嗪含量及制剂中5-HMF,过程简便、灵敏、准确。为该药提供了切实可行的质控方法。     

HPLC法测康妇灵滴丸中盐酸小檗碱的含量

目的建立用高效液相色谱法测定康妇灵滴丸中盐酸小檗碱含量的方法。方法采用HPLC法,AlltimaC18柱(4.6 mm×250 mm),流动相:0.1%磷酸溶液-乙腈(50∶50),流速:1.0 ml·min-1,检测波长:265 nm,柱温:30℃。结果盐酸小檗碱浓度范围在10.08～100.8 mg·L-1之间峰面积(S)与浓度(C)线性关系良好。结论该法可用于康妇灵滴丸的质量控制。     

HPLC法和UV法测定盐酸西替利嗪片含量的比较研究

目的:建立HPLC法测定盐酸西替利嗪片含量,与法定UV法相比较。方法:色谱柱Agilent C18柱(150 mm×4．6 mm,5μm),流动相:0．1 mol·L-1磷酸二氢钠溶液(用磷酸调pH值至3．7)-乙腈(60:40),流速1．0 ml·min-1,检测波长230 nm。结果:盐酸西替利嗪的线性范围为10．75-215μg·ml-1,平均回收率100．1％(RSD=0．4％,n=6)。结论:UV法片剂中辅料干扰测定,而HPLC法简便,准确,辅粒不干扰测定。     

高效液相色谱法测定厄贝沙坦缓释片的含量

目的建立测定厄贝沙坦缓释片中厄贝沙坦的含量的HPLC法.方法采用Diamonsil C18柱(250mm×4.6mm,5μm),以乙腈-0.02 mol·L-1磷酸二氢钾溶液(用磷酸调节pH至2.60)(45∶55)为流动相,流速1.0ml·min-1,245nm波长处检测.结果线性范围为12.4～185.4μg·ml-1(r=0.9999);平均回收率为100.1%,RSD为0.5%(n=9).结论本法操作简便、分析快速准确.     

高效液相色谱法测定杜仲缓释滴丸中绿原酸含量

目的建立测定杜仲缓释滴丸中绿原酸含量的高效液相色谱（HPLC）法。方法以迪马C18柱（250mm×4．6mm,5μm）为色谱柱,乙腈-0．4％磷酸溶液（13：87）为流动相,流速为1．0mL／min,检测波长为327nm。结果绿原酸质量浓度在1．3～130．0μg／mL范围内与峰面积值线性关系良好,r=0．9999（n=6）。结论HPLC法操作简便,结果准确可靠。     

HPLC-PAD法同时测定精制银翘解毒胶囊中对乙酰氨基酚、绿原酸、连翘苷和牛蒡苷的含量

目的:采用HPLC-PAD法同时测定精制银翘解毒胶囊中对乙酰氨基酚、绿原酸、连翘苷和牛蒡苷的含量.方法:色谱柱:Capcell Pak C18(150 mm×4.6 mm,5μm);流动相:乙腈-水(含0.25％的冰醋酸)梯度洗脱;检测波长:300 nm和228 nm;流速:1mL· min-1;柱温:30C.结果:对乙酰氨基酚测定的线性范围28.15～84.45 μg (r=0.9999),平均含量为235.06 mg·g-1,RSD为0.17％;绿原酸测定的线性范围0.2048～0.6144 μg (r=0.9998),平均含量为1.91 mg·g-1,RSD为0.21％;连翘苷测定的线性范围0.1054～0.3162μg (r=0.9994),平均含量为1.00 mg·g-1,RSD为0.32％;牛蒡苷测定的线性范围1.044～3.132 μg (r=0.9998),平均含量为7.04 mg·g-1,RSD为0.16％.结论:该法简便、灵敏、准确,适用于精制银翘解毒胶囊的质量控制.     

HPLC同时测定人参强心滴丸中华蟾酥毒基和脂蟾毒配基的含量

目的:建立测定人参强心滴丸中华蟾酥毒基和脂蟾毒配基含量的HPLC方法。方法:采用Diamonsil C18(200 mm×4.6 mm,5μm)色谱柱,流动相为0.5%磷酸二氢钾溶液-乙腈(45∶55,用磷酸调节pH为3.2),流速1.0 mL·min-1,检测波长为296 nm,柱温为室温。结果:华蟾酥毒基、脂蟾毒配基线性范围分别为2.54～50.8μg·mL-1(r=0.9999)和2.48～49.6μg·mL-1(r=0.9999),平均回收率(n=6)分别为99.9%(RSD=1.0%)和99.5%(RSD=0.59%)。结论:本法简便准确,专属性强,可作为人参强心滴丸中华蟾酥毒基和脂蟾毒配基含量的控制方法。     

UPLC测定红毛五加嫩叶中的绿原酸

目的 采用UPLC测定红毛五加嫩叶试制品中绿原酸的含量并比较差异.方法 Acquity UPLC(R)BEH C18柱(50 mm× 2.1 mm,1.7 μm),柱温30℃,流动相为乙腈-2‰磷酸溶液(10∶90),检测波长327 nm,流速0.2 mL· min-1.结果 绿原酸0.02 ～0.72 mg· mL-1与峰面积具有良好的线性关系,回归方程为:Y=3×107X-9.9481×104(r2 =0.9997,n=9),平均回收率为97.7％,RSD =0.61％(n=6),红毛五加嫩叶晒干品中绿原酸的含量最高(0.0326 g·g-1),百合粉中绿原酸含量为0.结论 所用方法简便、准确、重复性好,能为红毛五加嫩叶的开发提供参考.     

HPLC法测定注射用磷酸川芎嗪中主药的含量

目的:建立以高效液相色谱法测定注射用磷酸川芎嗪中主药含量的方法。方法:色谱柱为Zorbax Extend C18(150mm×4.6mm,5μm),流动相为甲醇-水(3∶2),检测波长为295nm。结果:磷酸川芎嗪检测浓度在0.21～3.00mg.mL-1范围内与峰面积积分值呈良好的线性关系(r=0.9999);平均回收率为100.1%,RSD=0.93%(n=9)。结论:本方法简便、准确、灵敏度高、重现性好,可用于注射用磷酸川芎嗪的质量控制。     

RP-HPLC法测定复方辛伐他汀烟酸缓释片中辛伐他汀的含量

目的采用RP-HPLC法,建立复方辛伐他汀烟酸缓释片中辛伐他汀含量的测定方法。方法色谱条件:Welch-C18色谱柱(4.6mm×33mm,3μm),以乙腈-0.1%磷酸溶液(50∶50)为流动相A,0.1%磷酸的乙腈溶液为流动相B进行梯度洗脱,流速为3.0mL·min-1;检测波长为238nm。结果辛伐他汀在19.99～999.6μg·mL-1范围内线性关系良好(r=0.9999),平均回收率为99.7%,(RSD=0.45%),定量限为27ng。结论该方法简单易操作,准确度好,专属性强,可用于辛伐他汀的含量测定。     

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.     

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.     

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.