同时测定小儿咳喘灵颗粒中4种成分的方法研究

目的：建立同时测定小儿咳喘灵颗粒中（R,S）-告依春、绿原酸、甘草苷和木犀草苷含量的方法。方法：采用高效液相色谱法,Inertsil C8-3色谱柱（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.5%乙酸溶液,梯度洗脱;流速：0.6 mL·min^-1;DAD检测器,检测波长：木犀草苷327 nm、绿原酸327nm、甘草苷276 nm、（R,S）-告依春245 nm。结果：金银花中木犀草苷和绿原酸、甘草中甘草苷及板蓝根中（R,S）-告依春在各自的线性范围内与其峰面积呈良好的线性关系;平均加样回收率在99.4%~103.4%范围内,RSD均符合规定。结论：该方法准确、简便、快速,可用于小儿咳喘灵颗粒中多味药材的多个活性成分的含量测定。     

双波长HPLC同时测定小儿咳喘灵颗粒中8种有效成分的含量

目的 采用HPLC同时测定小儿咳喘灵颗粒中盐酸麻黄碱、盐酸伪麻黄碱、（R,S）告依春、绿原酸、苦杏仁苷、甘草苷、木犀草苷、甘草酸的含量。方法 采用双波长HPLC,以Agilent ZORBAX SB-C₁₈色谱柱（4.6 mm×250 mm,5 μm）进行分离;流动相：0.1%磷酸水溶液-乙腈梯度洗脱;流速1 mL·min^-1;柱温30℃;检测波长210 nm（盐酸麻黄碱、盐酸伪麻黄碱、苦杏仁苷、甘草苷、木犀草苷）,245nm[（R,S）告依春、绿原酸、甘草酸]。结果 8种成分的峰面积与质量浓度的线性关系良好,加样回收率96.23%~100.7%。结论 该方法简便、快速、准确,可用于小儿咳喘灵颗粒的质量控制。     

HPLC法同时测定小儿咳喘灵颗粒中6种成分

摘 要 目的：建立利用HPLC法采取波长变换同时测定小儿咳喘灵颗粒中盐酸麻黄碱、（R,S） 告依春、苦杏仁苷、绿原酸、甘草苷、甘草酸含量的方法。方法: 色谱条件：Agilent Eclipse XDB C18（250 mm×4.6 mm,5 μm）,以乙腈 0.1%磷酸为流动相,梯度洗脱,流速为1.0 ml·min^-1 ,测定波长为207 nm（盐酸麻黄碱、苦杏仁苷）、237 nm（甘草酸、甘草苷、绿原酸）、245 nm[（R,S） 告依春）]。结果:盐酸麻黄碱进样浓度在2.423～96.920 μg·m^-1 范围与峰面积线性关系良好,r=0.999 2,平均回收率为100.1%(RSD=0.30%,n=6);（R,S） 告依春进样浓度在1.920～76.798 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为99.86%(RSD=1.14%,n=6);绿原酸进样浓度在2.396～92.891 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为98.57%(RSD=0.75%,n=6);苦杏仁苷进样浓度在1.982～79.279 μg·m^-1 范围与峰面积线性关系良好, r=0.999 8,平均回收率为99.67%(RSD=0.59%,n=6);甘草苷进样浓度在2.136～85.440 μg·m^-1 范围与峰面积线性关系良好, r=0.999 9,平均回收率为98.57%(RSD=0.69%,n=6);甘草酸进样浓度在2.432～97.260 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为98.57%(RSD=0.11%,n=6)。结论:该方法准确、重复性好,可用于小儿咳喘灵颗粒的质量控制。     

HPLC法同时测定肝炎康复丸中6种成分的含量

摘 要 目的：建立HPLC波长切换联合梯度洗脱法同时测定肝炎康复丸中6种主要成分[(R,S) 告依春、丹酚酸B、丹参酮ⅡA、木犀草苷、对羟基苯乙酮、滨蒿内酯]的含量。方法: 色谱柱为Agilent TC C18柱（250 mm×4.6 mm,5 μm）,流动相为乙腈 0.1%磷酸溶液梯度洗脱,流速为0.9 ml·min^-1,检测波长分别为245 nm[检测(R,S) 告依春]、270 nm（检测丹酚酸B和丹参酮ⅡA）、348 nm（检测木犀草苷）、278 nm（检测对羟基苯乙酮和滨蒿内酯）,柱温为25℃,进样量为10 μl。 结果:(R,S) 告依春、丹酚酸B、丹参酮ⅡA、木犀草苷、对羟基苯乙酮、滨蒿内酯的线性范围分别为1.99～49.75 μg·mL^-1 (r=0.999 9)、18.66～466.50 μg·mL^-1 (r=0.999 4)、2.25～56.25 μg·mL^-1 (r=0.999 8) 、2.62～65.50 μg·mL^-1 (r=0.999 8)、2.48～62.00 μg·mL^-1(r=0.999 2) 和2.55～63.75 μg·mL^-1 (r=0.999 6),平均加样回收率分别为98.42%、99.56%、97.96%、96.84%、98.10%和97.82%,RSD分别为0.83%、1.04%、1.53%、0.78%、1.44%和1.34%(n=6) 。 结论:本方法简便、准确、重复性好,可为肝炎康复丸多指标定量质量评价提供依据。     

HPLC同时测定四季三黄片中芦荟大黄素、黄芩苷、黄柏酮和西红花苷-I的含量

目的 采用HPLC同时测定四季三黄片中芦荟大黄素、黄芩苷、黄柏酮和西红花苷-I的含量。方法 采用welch Topsil-C₁₈色谱柱(4.6 mm×250 mm,4 μm);流动相：甲醇-0.2%磷酸水溶液;梯度洗脱;检测波长分别为254 nm(芦荟大黄素、黄芩苷、黄柏酮)和440 nm(西红花苷-I);流速：1.0 mL·min^-1;柱温：30 ℃。结果 芦荟大黄素、黄芩苷、黄柏酮和西红花苷-I线性范围分别为0.079 10~1.582 μg·mL^-1(r=0.999 5),0.167 5~3.350 μg·mL^-1(r=0.999 8),0.097 92~1.958 μg·mL^-1(r=0.999 7)和0.033 57~0.671 5 μg·mL^-1(r=0.999 4),平均加样回收率分别为95.9%(RSD=0.7%),97.5%(RSD=0.8),96.4%(RSD=1.0%),95.5%(RSD=1.3%)。结论 该方法简便、准确、专属性强、重复性好,可用于四季三黄片中芦荟大黄素、黄芩苷、黄柏酮和西红花苷-I的定量分析。     

双波长HPLC法同时测定复方肤清洗剂中3种指标性成分含量

摘 要 目的：建立双波长HPLC法同时测定复方肤清洗剂中绿原酸、咖啡酸、芍药苷3种指标性成分含量的方法。方法: 采用Inertsil C18柱（250 mm×4.6 mm,5 μm）为色谱柱,柱温40℃,以乙腈-0.02%磷酸水溶液（17∶83）为流动相,流速为1.0 ml·min^-1,检测波长分别为323 nm、230 nm。结果:绿原酸、咖啡酸和芍药苷分别在7.50~120.00 μg·mL^-1,2.50~40.00 μg·mL^-1,14.06~225.00 μg·mL^-1范围内线性关系良好,r分别为0.999 9,0.999 8,0.999 7;平均加样回收率分别为98.55%,94.52%,99.18%,RSD分别为1.66%,0.98%,0.65%（n=6）。结论:该方法简便快捷、结果准确、专属性强,可用于复方肤清洗剂的质量分析与控制。     

HPLC同时测定芍苓消银片中芍药苷、落新妇苷、绿原酸、迷迭香酸和甘草酸的含量

目的 建立同时测定芍苓消银片中芍药苷、落新妇苷、绿原酸、迷迭香酸和甘草酸含量的HPLC。 方法 采用Diamonsil C₁₈(250 mm×4.6 mm,5 μm)色谱柱,流动相为乙腈(A)-0.1%甲酸(B)系统,梯度洗脱;多种波长下同时检测。结果 芍药苷、落新妇苷、绿原酸、迷迭香酸和甘草酸的保留时间依次为44.2,57.5,28.6,72.3,90.6 min,回归方程依次为：y=33 605 228x-124 483,r=0.999 9,线性范围为3.25~60.5 μg·mL^-1;y=101 354 460x-100 4,r=0.999 9,线性范围为6.5~130 μg·mL^-1;y=119 599 014x+22 521,r=1.000 0,线性范围为0.98~19.6 μg·mL^-1;y=104 333 261x-365 9,r=0.999 9,线性范围为0.75~15 μg·mL^-1;y=24 700 178x+7 185,r=0.999 9,线性范围为8~160 μg·mL^-1。平均加样回收率依次为98.7%,100.4%,99.6%,102.1%,102.3%,RSD依次为为2.17%,0.74%,2.64%,1.39%,1.93%。结论 本方法操作较为简便,测定结果准确可靠,重复性好,能排除其他成分的干扰,可用于该制剂的质量控制。     

HPLC同时测定冠心康颗粒中芍药苷、丹酚酸B和羟基红花黄色素A的含量

目的 建立同时测定冠心康颗粒中芍药苷、丹酚酸B和羟基红花黄色素A含量的方法。方法 采用Welchrom C₁₈色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.1%磷酸(B)为流动相,梯度洗脱;流速：1.0 mL·min^-1;检测波长：230 nm。结果 芍药苷在7.02~52.64 μg·mL^-1内呈良好的线性关系(r=0.999 7),平均回收率为99.3%,RSD为1.2%;丹酚酸B在23.19~173.90 μg·mL^-1内呈良好的线性关系(r=0.999 7),平均回收率为98.2%,RSD为1.1%;羟基红花黄色素A在4.47~ 33.50 μg·mL^-1内呈良好的线性关系(r=0.999 3),平均回收率为98.0%,RSD为1.0%。结论 本法简便、灵敏、准确、重复性好,可用于冠心康颗粒的质量控制。     

HPLC同时测定黄石感冒片中阿魏酸、芦丁、大黄酸、大黄素和大黄酚的含量

目的 建立HPLC同时测定黄石感冒片中阿魏酸、芦丁、大黄酸、大黄素和大黄酚的含量。方法 采用HPLC,色谱柱为Welch Topsil-C₁₈柱(4.6 mm×250 mm,4 μm);以甲醇-0.1%磷酸溶液(78∶22)为流动相;流速：1.0 mL·min^-1;柱温：30 ℃;检测波长：280 nm。结果 阿魏酸、芦丁、大黄酸、大黄素和大黄酚峰线性范围分别为0.020 82~0.416 3 μg·mL^-1(r=0.999 7),0.011 32~0.278 3 μg·mL^-1(r=0.999 3),0.017 22~0.344 3 μg·mL^-1(r=0.999 5),0.015 79~0.315 8 μg·mL^-1(r=0.999 6)和0.051 34~1.027 μg·mL^-1(r=0.999 9),平均加样回收率分别为97.4%(RSD=1.1%),95.0%(RSD=0.88%),97.5%(RSD=1.3%),97.4%(RSD=1.4%)和96.3%(RSD=0.87%)。结论 新建方法简便、准确,可用于黄石感冒片的定量分析方法。     

HPLC同时测定依折麦布辛伐他汀片中两种成分的含量

目的 建立高效液相色谱法同时测定依折麦布辛伐他汀片中依折麦布和辛伐他汀的含量。方法 色谱柱Phenomenex Luna Phenyl Hexyl(4.6 mm×150 mm,5 μm),以乙腈-0.02 mol·L^-1磷酸二氢钠(pH 4.5)为流动相,梯度洗脱,流速1.0 mL·min^-1,检测波长231 nm,柱温30 ℃。结果 依折麦布在10.0~100.0 μg·mL^-1内线性关系良好(r=0.999 8),辛伐他汀在20.0~200.0 μg·mL^-1内线性关系良好(r=0.999 9)。依折麦布的平均回收率为99.5%,RSD为1.3%(n=9),辛伐他汀的平均回收率为99.8%,RSD为0.9%(n=9)。结论 本方法简便、可靠、准确度高、重复性好,可用于同时测定依折麦布辛伐他汀片中的依折麦布和辛伐他汀的含量。     

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.     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.     

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.