高效液相色谱法同时测定肺力咳合剂中苯甲酸钠等6种防腐剂含量

目的：建立高效液相色谱（HPLC）同时测定肺力咳合剂中苯甲酸钠等6种防腐剂含量的方法。方法：采用HPLC,色谱柱为Agilent XDB-C18色谱柱（250 mm×4.6 mm,5 μm）,流动相：甲醇-0.025 mol/L磷酸二氢钠溶液（梯度洗脱）;流速：1.0 mL/min;柱温30 ℃,检测波长228 nm、255 nm。结果：肺力咳合剂中苯甲酸钠在0.063 54～211.800 00 μg（r=0.999 9）、山梨酸钾在0.066 06～220.200 00 μg（r=0.999 9）、对羟基苯甲酸甲酯在0.062 70～209.000 00 μg（r=0.999 9）、对羟基苯甲酸乙酯在0.066 12～220.400 00 μg（r=0.999 9）、对羟基苯甲酸丙酯在0.067 98～226.600 00 μg（r=0.999 9）,对羟基苯甲酸丁酯在0.063 30～211.000 00 μg（r=0.999 9）范围内线性良好,平均回收率分别为100.72%（RSD=0.82%）、104.82%（RSD=1.59%）、101.11%（RSD=0.25%）、102.39%（RSD=1.33%）、102.56%（RSD=1.35%）、101.09%（RSD=0.34%）。10批样品中均未检出山梨酸钾、对羟基苯甲酸甲酯、对羟基苯甲酸丁酯,苯甲酸钠、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯的含量分别为2.132 6~2.602 6 mg/mL、0.110 8~0.126 0 mg/mL、0.399 9~0.408 9 mg/mL。结论：该方法具有操作简单,专属性强,准确度高的优点,可以更全面的控制肺力咳合剂中防腐剂的含量。     

HPLC法同时测定小儿咳喘灵口服液中7种防腐剂的含量

摘要：目的:建立HPLC法同时检测小儿咳喘灵口服液中苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯、对羟基苯甲酸异丁酯等7种防腐剂的含量方法。方法:采用Agilent ZORBAX SB-phenyl（250mm×4.6 mm,5μm）色谱柱,以乙腈-0.2%磷酸溶液为流动相,梯度洗脱,流速1 ml·min-1,检测波长分别为230 nm和255 nm。结果:7种防腐剂在0.5～20μg·ml-1线性范围内均呈良好线性关系（r>0.999）。平均回收率为102.3%～103.3%,RSD 0.3%～0.4%（n=6）。检出限（LODs,S/N≥3）为0.01～0.03μg·ml-1。结论:该方法简便、准确、重复性好,可用于小儿咳喘灵口服液中防腐剂限量的测定。     

HPLC法同时测定氢溴酸右美沙芬糖浆中 主药和降解杂质及防腐剂的含量

目的：建立同时测定氢溴酸右美沙芬糖浆中主成分氢溴酸右美沙芬、杂质5-羟甲基糠醛及防腐剂苯甲酸、羟苯乙酯含量的高效液相色谱方法。方法：色谱柱为Phenomenex Luna C18（250 mm × 4.6 mm,5 μm）,流动相为甲醇-0.1 mol·L-1磷酸二氢铵溶液,梯度洗脱,体积流量为1.0 mL·min-1,柱温为30 ℃,检测波长为279 nm,进样体积为20 μL。结果：氢溴酸右美沙芬、5-羟甲基糠醛、苯甲酸、羟苯乙酯的线性范围分别为29.21～876.2、1.94～58.29、27.08～812.4、5.85～175.4 μg·mL-1（r≥0.9997）。4种成分的平均加样回收率分别为99.23%、98.86%、100.3%、98.51%,RSD分别为1.03%、1.52%、1.11%、1.64%（n=6）。结论：该方法简便、准确,可用于测定氢溴酸右美沙芬糖浆中氢溴酸右美沙芬、5-羟甲基糠醛、苯甲酸和羟苯乙酯的含量。     

MEKC法同时测定小儿止咳糖浆中6种防腐剂的含量

摘要：目的:建立胶束高效毛细管电泳（MEKC）同时测定小儿止咳糖浆中苯甲酸、山梨酸、羟苯甲酯、羟苯乙酯、羟苯丙酯、羟苯丁酯的方法。方法:采用胶束电动毛细管分离模式,用未涂渍的标准熔融石英毛细管柱（75μm×50 cm,42 cm）为分离通道;分离缓冲液为15 mmol·L-1Na2B4O7-H3BO-3溶液(p H 8. 7,含50 mmol·L-1SDS);检测波长195 nm;运行电压:15 k V;柱温度:25℃;压力进样:50 mbar,5s。结果:6种防腐剂在各自浓度的范围内线性关系良好（r=0. 999 3～0. 999 8）,平均加样回收率在97. 1%～102. 2%范围内,RSD均小于2. 0%（n=9）。11家企业共22批样品中苯甲酸的含量均符合规定,其余5种防腐剂未检出。结论:本方法专属性强,准确度高,重复性良好,可用于小儿止咳糖浆中防腐剂的检测,为其生产工艺和质量控制提供参考依据。     

HPLC法测定小儿白贝止咳糖浆中原阿片碱的含量

目的：建立小儿白贝止咳糖浆中原阿片碱的含量测定方法。方法：采用高效液相色谱法测定，色谱条件为：Agilent TC C18 色谱柱(250mm×4.6 mm，5 μm)，流动相为乙腈-三乙胺醋酸溶液（18 : 82），流速1 mL? min-1，检测波长289 nm，柱温30 ℃。结果：原阿片碱在0.1395～2.2323 μg范围内线性关系良好（r = 0.999 8），平均回收率99.14 %（RSD=0.82 %）。3批样品含量测定结果：平均含量为6.6 μg?mL-1。结论：本方法简便、准确、重现性好，可以作为小儿白贝止咳糖浆的控制方法。     

HPLC法同时测定宣肺止咳糖浆中盐酸麻黄碱和苦杏仁苷的含量

目的：建立高效液相色谱法同时测定宣肺止咳糖浆中盐酸麻黄碱和苦杏仁苷含量的方法.方法：采用Luna C18柱（250 mm×4.6 mm,5 μn）,乙腈-0.1%磷酸溶液（加入0.1%三乙胺）（10：90）为流动相,流速1.0 ml·min-1,检测波长210 nm,柱温30℃.结果：盐酸麻黄碱在2.2～111.5μg·ml-1的范围内有良好的线性关系,r=0.999 6,平均回收率为96.4%,RSD为1.34%（n=9） 苦杏仁苷在20.4～1 020.0μg·ml-1范围内有良好线性关系,r=0.999 9,平均回收率为99.0%,RSD为0.50%（n=9）.结论：方法可同时测定盐酸麻黄碱和苦杏仁苷的含量,简便,准确,重复性好,可作为宣肺止咳糖浆的质量控制.     

HPLC法测定小儿白贝止咳糖浆中原阿片碱的含量

目的：采用高效液相色谱法测定小儿白贝止咳糖浆中原阿片碱的含量。方法：色谱柱：Bonchromc18（250mm×4．6mm,5μm）;流动相：乙腈-0．4％磷酸（20：80）;检测波长：289nm。结果：原阿片碱进样量在0．087～0．870μg范围内,呈良好的线性关系（r=0．9999）。平均加样回收率为98．8％,RSD=0．84％（n=6）。结论：方法易于操作,结果准确,重复性良好,可用于小儿白贝止咳糖浆的质量控制。     

HPLC法测定羟苯乙酯中对羟基苯甲酸的含量

摘 要 目的：建立羟苯乙酯中特定杂质对羟基苯甲酸的含量测定方法。 方法: 采用Waters C18（250 mm×4.6 mm, 5 μm）色谱柱,以甲醇 1%冰醋酸（60∶40）为流动相,流速1.0 ml·min-1,柱温30℃,检测波长254 nm,进样量为20 μl。结果: 在该色谱条件下,羟苯乙酯和对羟基苯甲酸能完全分离;对羟基苯甲酸在0.021 8~6.526 8 μg·ml-1的浓度范围线性关系良好（r=0.999 9）;平均回收率为100.23%（RSD=0.45%, n=6）。 结论: 本方法准确度高、重复性好,可用于羟苯乙酯中对羟基苯甲酸的测定。     

HPLC法测定桉叶止咳糖浆中黄芩苷与麻黄碱的含量

目的建立HPLC法测定桉叶止咳糖浆中黄芩苷与麻黄碱的含量。方法黄芩苷采用PE-Rack C18（5umm,150mm×4.6mm）色谱柱,以0.1%磷酸溶液-甲醇（58：42）为流动相,流速为1.0ml.min-1,检测波长为277nm,柱温为30℃。麻黄碱采用Diamonsil C18（5μm,250×4.6mm）色谱柱,以0.1%磷酸溶液（含0.1%三乙胺）-乙腈（97：3）为流动相,流速为1.0mL.min-1,检测波长为205nm,柱温为25℃。结果黄芩苷在2.8～90μg.ml-1范围内呈良好的线性关系（R2=0.9998）,平均回收率为99.1%,RSD=1.72%（n=6）;麻黄碱在0.1513～2.0716μg范围内线性关系良好（R2=1.0000）,平均回收率为99.43%,RSD=1.10%（n=6）。结论结果表明本方法测定桉叶止咳糖浆中黄芩苷与麻黄碱的含量灵敏度高,操作简便、准确,重现性好。     

高效液相色谱法测定小儿百部止咳糖浆中橙皮苷的含量

［摘要］目的 建立小儿百部止咳糖浆中橙皮苷的含量测定方法. 方法 采用高效液相色谱法,色谱柱：Kromasil C18（4.6 mm×250 mm,5 μm）;流动相：甲醇-水-醋酸（35：61：4）;流速：1 mL·min^-1;检测波长：283 nm;以外标法测定. 结果 橙皮苷在0.444～2.220 μg范围内,橙皮苷进样量与峰面积值呈良好的线性关系（r＝0.999 9）.橙皮苷的平均回收率为99.68 %,RSD为0.95%. 结论 该法操作简便,结果可靠,为小儿百部止咳糖浆限量标准提供了科学依据.     

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.     

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.     

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.