HPLC-ELSD法测定注射用益气复脉(冻干)中钠元素

目的 建立一种用于测定注射用益气复脉（冻干）中钠元素含量的方法。方法 采用强阳离子交换色谱柱（SCX）,以0.05 mol/L乙酸铵（乙酸调节pH至4.8）-乙腈（50：50）为流动相,体积流量为1.0 mL/min,柱温30℃,撞击器“关闭”模式,漂移管温度为90℃,压缩空气流量为2.5 L/min,检测器的增益值为1。结果 钠元素在60～180 μg/mL范围内线性良好（r＝0.999 3）;准确度试验（n＝9）平均回收率为90.4%,RSD为1.8%;注射用益气复脉（冻干）中钠元素质量分数均值为0.48%（0.33%～0.55%）。结论 所建立的方法简单可靠,可用于测定注射用益气复脉（冻干）中钠元素的含量测定。     

HPLC法测定肌瘤化消颗粒中淫羊藿苷和丹参酮ⅡA

目的 建立测定肌瘤化消颗粒中淫羊藿苷和丹参酮II_A的HPLC法。方法 采用高效液相色谱法,Diamonsil^TM C₁₈色谱柱（250 mm×4.6 mm,5 μm）;流动相：乙腈-水,梯度洗脱;检测波长为270 nm;柱温为40℃;体积流量为1.0 mL/min;进样量10 μL。结果 淫羊藿苷在7.5～50 μg、丹参酮II_A在3～20 μg与峰面积的线性良好（r=0.999 9）。平均回收率分别为100.2%、100.1%,RSD值分别为0.9%、1.3%（n=9）。结论 本法操作简便,重现性好,可有效控制肌瘤化消颗粒的质量。     

HPLC法测定麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的 建立麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定方法。方法 采用高效液相色谱（HPLC）法,色谱柱：Wondasil C₁₈（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.1%磷酸溶液（5：95）;流速：1 ml/min;检测波长：215 nm;柱温：30℃;进样量：10 μl。结果 盐酸麻黄碱、盐酸伪麻黄碱的质量浓度分别在4.231~42.31 μg/ml（r=0.999 7）、1.187~11.87 μg/ml（r=0.999 9）范围内与各自峰面积线性关系良好,平均加样回收率为分别为98.9%、98.1%;RSD分别为0.48%、0.64%。结论 该法准确度高、重复性好, 可用于麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定。     

HPLC法测定山楂红曲胶囊中洛伐他汀

目的 建立山楂红曲胶囊中洛伐他汀的处理及含量测定方法。方法 色谱柱为Kromasil C₁₈柱（250 mm×4.6 mm,5μm）,紫外检测波长238 nm,柱温25℃,体积流量1.0 mL/min,流动相为甲醇：0.1%磷酸溶液（75：25）。结果 洛伐他汀质量浓度在2.04~306 μg/mL与峰面积线性关系良好,平均回收率为98.58%,RSD=1.12%（n=9）。结论 该方法准确、简便,可用于山楂红曲胶囊的质量控制。     

清眩软胶囊的质量控制研究

目的 建立清眩软胶囊的定性鉴别和定量测定方法。方法 采用TLC法对本方中的川芎、荆芥穗和薄荷进行定性鉴别;采用HPLC法对方中主要成分欧前胡素进行测定。Agilent C₁₈色谱柱（250 mm×4.6 mm,5 μm）;以乙腈-水（42.5：57.5）为流动相;检测波长300 nm,柱温为35℃,体积流量为1.5 mL/min。结果 薄层色谱斑点清晰,阴性样品无干扰。欧前胡素在1.09～54.55 μg/mL与峰面积呈良好的线性关系,平均回收率为97.0%,RSD值为0.77%（n=6）。结论 所建立的定性和定量方法结果可靠、准确,重现性好,无干扰,可用于清眩软胶囊的质量控制。     

双波长HPLC法测定止痒地霜中地塞米松和羟苯乙酯的含量

目的 建立双波长HPLC法同时测定止痒地霜中地塞米松磷酸钠和羟苯乙酯的含量。方法 采用RP-HPLC法,以Wondasil C₁₈（4.6 mm×250 mm,5 μm）为色谱柱,以三乙胺溶液-甲醇-乙腈（52：43：5）为流动相;检测波长为242 nm,流速为1.0 ml/min。结果 羟苯乙酯和地塞米松磷酸酯分别在21.42～64.26 μg/ml （r=1.0000）和20.84～62.53 μg/ml （r=0.9999）范围内有良好的线性关系,平均回收率分别为99.1%（RSD=0.41%）和99.0%（RSD=0.72%）。结论 该法简便、准确、重复性好,可用于止痒地霜的质量控制。     

用HPLC法同时测定自制复方特比萘酚软膏中3个主药成分的含量

目的 建立同时测定自制复方特比萘酚软膏中3个主药成分含量的HPLC法。方法 色谱柱为ZORBAX SB-C₈柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.1%磷酸溶液（70∶30）,柱温：30 ℃,流速：1.0 ml/min,检测波长：248 nm,进样量：10 μl。结果 盐酸特比萘芬在20.4～204.0 μg/ml（r =0.999 7）,莫匹罗星在40.4～404.0 μg/ml（r=0.9998）,糠酸莫米松在2.02～20.20 μg/ml（r=0.999 7）的浓度范围呈良好的线性关系,加样回收率分别为99.39%、99.21%、99.97%,RSD分别为0.82%、0.59%、0.81%（n=9）。结论 该方法的专属性、重复性良好,可用于自制复方特比萘酚软膏中的特比萘酚、莫匹罗星、糠酸莫米松的含量测定。     

阿糖胞苷在大鼠体内转化为阿糖尿苷的药动学研究

目的 建立测定大鼠血浆中阿糖尿苷的LC-MS/MS方法,用于大鼠尾iv注射用盐酸阿糖胞苷后阿糖尿苷在体内的药动学研究。方法 采用LC-MS/MS法。ACQUITY UPLC BEH C₁₈色谱柱（50 mm×2.1 mm,1.7 μm）;流动相：水–乙腈,梯度洗脱;体积流量：0.2 mL/min;柱温：40 ℃;进样量：5 μL。离子源：ESI源;扫描方式：多反应监测（MRM）方式,扫描时间为0.1 s;毛细管电压：2.5 kV;锥孔电压：26 V;离子源温度：110 ℃;去溶剂气温度：350 ℃;去溶剂气流量：500 L/h;锥孔气流量：50 L/h。采用回归方程计算血浆中阿糖尿苷。SD大鼠尾iv注射用盐酸阿糖胞苷,制备血药质量浓度–时间曲线,计算药动学参数。结果 阿糖尿苷在1.0～1 000 ng/mL线性关系良好,日内、日间RSD值均小于15%,准确度在±15%,平均提取回收率在90%以上,基质效应在97.3%,稳定性良好。药动学参数：t_max是1.0 h,C_max是134.2 ng/mL,AUC_0-t是2 316.0 ng•h/mL,t_1/2是4.3 h。结论 该方法适合大鼠尾iv阿糖胞苷后阿糖尿苷在体内的药动学研究。     

HPLC法测定六味地黄胶囊中的毛蕊花糖苷、马钱苷、芍药苷和丹皮酚

目的 建立同时测定六味地黄胶囊中毛蕊花糖苷、马钱苷、芍药苷和丹皮酚4种成分含量的高效液相色谱（HPLC）测定方法。方法 应用HPLC-梯度洗脱法,采用Kromasil C₁₈（250 mm×4.6 mm,5 μm）色谱柱,以1%冰醋酸为流动相A,乙腈为流动相B进行梯度洗脱,体积流量为1.0 mL/min,检测波长为230 nm。结果 毛蕊花糖苷、马钱苷、丹皮酚和芍药苷测定浓度的线性范围分别为6～60、15～150、50～500 μg/mL和5～50 μg/mL,r值均大于0.999,平均加样回收率分别为98.3%、99.3%、99.0%和99.0%,相对标准偏差（RSD）值均小于0.9%（n=9）。结论 该实验方法简便、结果准确,可有效地用于六味地黄胶囊的质量控制。     

HPLC测定安尔眠胶囊中2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷

目的 建立安尔眠胶囊中2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷（C₂₀H₂₂0₉）的含量测定方法。方法 采用高效液相色谱（HPLC）法,以Dionex Acclaim 120^® C₁₈色谱柱（150 mm×4.6 mm,5 μm）为分离柱,以乙腈-1%甲酸溶液（23：77）为流动相,体积流量1.0 mL/min,检测波长320 nm,柱温25 ℃。结果 2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷在0.010～0.200 μg呈现良好的线性关系（r=0.999 6）,平均回收率为97.35%,RSD为2.07%。结论 该方法<准确可靠,适用于安尔眠胶囊中2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的含量测定。     

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.