RP-HPLC法测定人血中盐酸伪麻黄碱浓度

目的建立反相高效液相色谱法测定盐酸伪麻黄碱的血药浓度。方法血浆中盐酸伪麻黄碱经碱化有机萃取后,用稀盐酸反相萃取后分析,色谱柱Nova-pakC18(150×3.9mm,4μm),柱温25℃,流动相为甲醇-0.5%硫酸铵(5∶95,硫酸调节pH至3.0,v/v),流速:0.9mL.min-1,检测波长210nm,盐酸苯丙醇胺(phenylpropanolamine hydrochloric,PPA)为内标。结果盐酸伪麻黄碱在28.5~1140ng.mL-1浓度范围内相关系数为0.9992(n=6),平均回收率为100.5%,日内及日间RSD均小于2.2%(n=5),最低检测限为9.5ng.mL-1。结论本法可用于盐酸伪麻黄碱血药浓度测定。     

HPLC法同时测定氨麻苯美片中4种主要成分的含量

目的:建立同时测定氨麻苯美片中盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明等成分含量的HPLC方法。方法:色谱柱为Kromasil 60-5CN(25 mm×4.6 mm,5μm)柱;以乙腈-pH3.0的40 mmol.L-1三乙胺水溶液(20∶80)为流动相;检测波长为215 nm;流速为1.0 mL.min-1。结果:盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明的线性范围分别为6.036~150.9μg.mL-1(r=1.0000),65.42~1636μg.mL-1(r=0.9989),3.010~75.25μg.mL-1(r=1.0000),50.90~127.2μg.mL-1(r=1.0000);加样回收率(n=9)分别为98.5%,100.9%,99.1%和99.6%。结论:本法简单、快速、准确,可用于氨麻苯美片中4种主要成分的同时测定。     

LC-MS/MS测定人血浆中的盐酸伪麻黄碱

目的 采用LC-MS/MS法测定人血浆中盐酸伪麻黄碱的血药浓度.方法 血浆样品经液-液萃取,结合液-液反相萃取的方法处理,采用Diamonsil~(TM) C_(18)柱(150 mm ×4.6 mm,5μm),以甲醇-10 mmol·L~(-1)醋酸铵(冰醋酸调pH4)(20:80)为流动相,LC-MS/MS用正离子电喷雾离子源(ESI~+)、离子选择通道为盐酸伪麻黄碱(m/z 166→148)、磷酸可待因内标(m/z300→191).结果 盐酸伪麻黄碱血药浓度5.065～1.013×10~3ng·ml~(-1)与检测信号具有良好的线性关系(r=0.9986),最低定量浓度为1 ng·ml~(-1).低、次低、中、高浓度的盐酸伪麻黄碱的萃取回收率分别为86.86%±5.8%、95.24%±4.31%、96.91%±1.75%、92.60%±7.79%;内标的萃取回收率为86.24%±3.86%.盐酸伪麻黄碱的日内、日间RSD均小于11.7%.结论 所建方法适用于盐酸伪麻黄碱的生物等效性及药物动力学的研究.     

HPLC法测定西替伪麻缓释片含量

目的建立高效液相色谱法测定盐酸西替利嗪和盐酸伪麻黄碱含量的方法。方法采用ODS柱(150 mm×4.6 mm),以甲醇-0.05 mol.L-1磷酸二氢钾(70∶30)(每1 000 m l加入十二烷基硫酸钠0.3 g)为流动相,使用紫外检测器,于214 nm波长处测定。结果盐酸西替利嗪的线性范围在1.0~20.0 mg.L-1(r=0.9999),RSD=0.92%(n=9),盐酸伪麻黄碱的线性范围在24~480 mg.L-1(r=0.9999),RSD=0.92%(n=9),检测限分别为0.1μg和1.2μg。结论本法可对盐酸西替利嗪和盐酸伪麻黄碱进行同时测定,具有快速、简便、灵敏、准确的特点。     

HPLC法测定鼻炎糖浆中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的建立高效液相色谱法测定鼻炎糖浆中盐酸麻黄碱和盐酸伪麻黄碱含量的测定方法。方法采用Agilent Zorbax SB-C18色谱柱(4.6 mm×250 mm,5μm),乙腈-0.2%磷酸溶液(含0.2%三乙胺)(2∶98)为流动相,流速:1.0 m L·min-1,检测波长206 nm,柱温:25℃。结果盐酸麻黄碱进样量在0.124¹.86μg范围内与峰面积呈良好线性(r=0.999 9),平均回收率为99.99%,RSD=1.24%(n=6);盐酸伪麻黄碱进样量在0.103 81.86μg范围内与峰面积呈良好线性(r=0.999 9),平均回收率为99.99%,RSD=1.24%(n=6);盐酸伪麻黄碱进样量在0.103 8¹.557μg范围内与峰面积呈良好线性(r=0.999 9),平均回收率为99.33%,RSD=1.93%(n=6)。结论该方法准确、重复性好,可用于鼻炎糖浆中盐酸麻黄碱和盐酸伪麻黄碱的测定。     

蛤蚧定喘丸含量测定方法的改进

目的:改进《中国药典》2010年版蛤蚧定喘丸的含量测定方法。方法:采用高效液相色谱法同时测定盐酸麻黄碱和盐酸伪麻黄碱的含量,色谱柱为Waters SunFire C18柱(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%磷酸(4∶96),流量1.0 mL.min-1,检测波长207 nm,柱温25℃。结果:盐酸麻黄碱在0.025 1～0.502μg,盐酸伪麻黄碱在0.025 03～0.500 6μg范围内浓度与峰面积呈良好的线性关系(r=0.999 9),二者平均回收率(n=6)分别为100.3%(RSD=0.75%)、100.9%(RSD=0.79%)。结论:该方法简便、准确,重现性好,可同时测定盐酸麻黄碱和盐酸伪麻黄碱的含量,改进了2010年版《中国药典》该药品的质量控制方法。     

HPLC测定咖酚伪麻分散片中的3种成分

目的 采用HPLC法测定咖酚伪麻分散片中的对乙酰氨基酚、盐酸伪麻黄碱和咖啡因.方法 采用Diamonsil C<,18>色谱柱(150 mm×4.6 mm,5 μm),流动相为甲醇-0.05 mol·L<'-1>磷酸二氢钠溶液(20∶80),流速1.0 ml·min<'-1>,检测波长210nm.结果 对乙酰氨基酚、盐酸伪麻黄碱和咖啡因的线性范围分别为0.0532～1.3355 μg(r=0.9999)、0.0489～0.6110 μg(r=0.9999)和0.0232～0.2895 μg(r=0.9999),平均回收率分别为99.6%、99.7%、99.7%(n=9).结论 所建方法 分离效果好、灵敏度高、重复性好、准确可靠.     

高效液相色谱法测定氨麻美敏片3个组分含量方法的改进

目的 建立测定氨麻美敏片中盐酸伪麻黄碱、氢溴酸右美沙芬、马来酸氯苯那敏含量的高效液相色谱法.方法 采用Waters Xterra RP18柱(250mm×4.6 mm,5μm),流动相为乙腈-水-三乙胺(17:81.5:1.5),流速为1.0mL/min,检测波长210nm,柱温35℃.结果 盐酸伪麻黄碱、氢溴酸右美沙芬、马来酸氯苯那敏质量浓度分别在150～360μg/mL(r=0.9999),80～190 μg/mL(r=1.0000),1O～24μg/mL(r=1.0000)范围内与峰面积呈良好的线性关系,平均回收率分别为99.89%,99.92%,99.91%,RSD分别为0.73%,0.34%,0.35%(n=9),检测限分别为0.69,0.75,1.48 μg/mL.结论 该方法准确、简便,可用于氨麻美敏片中3个组分的的含量测定.     

高效液相色谱法测定人血浆中盐酸伪麻黄碱浓度

目的建立测定人血浆中盐酸伪麻黄碱浓度的方法。方法血浆样品经混合碱液碱化、甲基叔丁基醚萃取、0.5%盐酸溶液酸化反提处理后,采用反相HPLC法测定。色谱柱:Kromasil C18柱(250 mm×4.6 mm,5μm),柱温30℃;流动相:0.01 mol.L-1磷酸盐缓冲液(pH6.5)-乙腈(62∶38),流速1.0 m l.m in-1;检测波长210 nm。结果盐酸伪麻黄碱在0.015-1.60 mg.L-1范围内线性关系良好,回归方程为:Y=4631.8X 3.76(r=0.9998),该方法平均回收率为101.7%,日内RSD为3.41%~4.25%,日间RSD为6.47~9.66%。结论该法简便、灵敏、快速、稳定性好,可用于临床血药浓度检测及药代动力学研究。     

HPLC法测定小儿咳喘灵颗粒中盐酸麻黄碱和盐酸伪麻黄碱含量

目的建立高效液相色谱法同时测定小儿咳喘灵颗粒中盐酸麻黄碱和盐酸伪麻黄碱含量的方法。方法采用反相高效液相色谱法,色谱柱为Agilent-ODS-3(5μm,4.6 mm×250 mm),以乙腈-0.1%磷酸溶液(5∶95)为流动相;检测波长为207 nm,流速为1.0 ml.min-1,柱温25℃。结果盐酸麻黄碱线性浓度范围在0.0306~0.306μg,r=0.999 9,平均回收率为99.52%,RSD=0.39%(n=9),盐酸伪麻黄碱线性浓度范围在0.0278~0.278μg,r=0.999 8,平均回收率为99.49%,RSD=0.52%(n=9)。结论本法简单准确,重复性好,可作为小儿咳喘灵颗粒的质量控制方法。     

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.

---

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.     

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.     

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.     

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.