双波长HPLC法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立高效液相色谱法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯含量的方法.方法:色谱柱:CAPCELL PAK-C18柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(48:52);流速为1.0 ml·min-1;柱温:30℃;检测波长:225 nm(穿心莲内酯)、250 nm(脱水穿心莲内酯);进样量:5 μl.结果:穿心莲内酯在4.17～41.68 μg·ml-1 (r=0.999 9)、脱水穿心莲内酯在4.04～40.40 μg·ml-1(r=0.999 9)浓度范围内线性关系良好;穿心莲内酯回收率为99.21%(RSD=1.3%,n=6),脱水穿心莲内酯回收率98.73%(RSD=1.1%,n=6).结论:该方法简单、准确,可作为止痢宁片的质量控制.     

HPLC法测定莲芝消炎胶囊中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立反相高效液相色谱法测定莲芝消炎胶囊中穿心莲内酯和脱水穿心莲内酯含量的方法。方法:色谱柱为Kromasil-C_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(55:45),流速1.0ml·min~(-1),检测波长225 nm,柱温40℃。结果:穿心莲内酯在0.23～2.30μg范围内线性良好。r=0.999 8,平均加样回收率为100.40%,RSD 为2.13%;脱水穿心莲内酯在0.25～2.50μg范围内线性良好,r=0.999 8,平均加样回收率为101.8%,RSD 为2.0%。结论:该方法简便、准确、灵敏度高,可有效控制莲芝消炎胶囊的质量。     

HPLC法同时测定慢性盆腔炎灌肠液中穿心莲内酯和脱水穿心莲内酯的含量

目的建立用反相高效液相色谱法测定慢性盆腔炎灌肠液中穿心莲内酯和脱水穿心莲内酯含量的方法。方法色谱柱:Agielnt TC-C18(250mm×4.6mm,5μm);流动相:甲醇-水(52∶48);柱温:不设定;流速:1.0mL·min-1;检测波长:225nm(穿心莲内酯),254nm(脱水穿心莲内酯)。结果穿心莲内酯和脱水穿心莲内酯的回归方程为:A=22 274 C-49.395,r=0.999 8;A=15 904 C-3.691,r=0.999 6;线性范围分别为:0.020 58~0.205 8和0.008 328~0.083 28mg·mL-1。平均回收率分别为99.62%和100.12%;RSD分别为1.81%和2.05%。结论 HPLC法测定慢性盆腔炎灌肠液中穿心莲内酯和脱水穿心莲内酯的含量,具有专属性强、精密度好、操作简单、准确度高等特点。     

穿心莲药材及其制剂中6个内酯类成分的含量分析

目的:建立RP-HPLC法同时测定穿心莲药材及其制剂中6个主要内酯成分(穿心莲内酯、异穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯、脱水穿心莲内酯和穿心莲宁)的含量。方法:采用Kromasil RP-C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-水为流动相,采用二元梯度洗脱,流速1.0 mL.min-1,检测波长226 nm,柱温25℃。结果:穿心莲内酯、异穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯、脱水穿心莲内酯和穿心莲宁的线性范围分别为0.17～6.72μg(r=0.9970),0.04～1.67μg(r=0.9967),0.11～4.32μg(r=0.9964),0.11～4.32μg(r=0.9969),0.19～7.60μg(r=0.9965),0.03～1.24μg(r=0.9972);穿心莲药材平均加样回收率(n=6)分别为100.5%(RSD=2.3%),100.7%(RSD=2.9%),99.3%(RSD=2.1%),100.8%(RSD=3.0%),100.9%(RSD=3.0%),101.3%(RSD=2.7%)。结论:所建立的含量测定方法简便可行,重复性良好,可用于穿心莲药材及...     

HPLC法测定穿心莲滴丸中穿心莲内酯和脱水穿心莲内酯的含量

目的建立测定穿心莲内酯和脱水穿心莲内酯总含量的方法,用于穿心莲滴丸的质量控制。方法采用HPLC法。色谱柱:Diamonsil ODS柱(4.6 mm×250 mm,5μm),流动相:甲醇-水(体积比60∶40),流速:1.0 mL.min-1,检测波长:231 nm,柱温:35℃。结果穿心莲滴丸中穿心莲内酯、脱水穿心莲内酯与其他成分分离良好;穿心莲内酯的质量浓度在50.0~300.0 mg.L-1(r=0.999 8)内、脱水穿心莲内酯的质量浓度在20.0~120.0 mg.L-1(r=0.999 7)内与峰面积呈现良好的线性关系;穿心莲内酯、脱水穿心莲内酯的回收率分别为101.62%、97.72%,RSD分别为1.9%、2.1%。结论该方法可有效地控制穿心莲滴丸的质量。     

高效液相色谱法测定穿黄消炎片中穿心莲内酯和脱水穿心莲内酯的含量

目的建立HPLC测定穿黄消炎片中穿心莲内酯和脱水穿心莲内酯含量的方法。方法色谱柱为Dikma Di-amonsil C18柱(4.0 mm×250 mm,5μm),以甲醇-水(50∶50)为流动相,脱水穿心莲内酯检测波长254 nm、穿心莲内酯检测波长为225 nm;采用外标法定量。结果穿心莲内酯与脱水穿心莲内酯的线性范围内分别为2.928~146.4μg.mL-1和5.98~299μg.mL-1,相关系数r均为0.999 9;回收率分别为101.82%(RSD=2.2%)和97.52%(RSD=2.4%)。结论本方法操作简便、重现性好,适合于本制剂的含量测定。     

穿心莲胶囊质量控制

目的:通过研究,提高穿心莲胶囊质量标准。方法:采用高效液相色谱(HPLC)法同时测定脱水穿心莲内酯和穿心莲内酯的含量。(色谱柱:YMC Hydrosphere C18(250mm×4.6mm,5μm),乙腈-水(二元梯度洗脱)为流动相,流速为1mL.min-1,柱温为35℃,检测波长为254nm。结果:穿心莲内酯的线性范围为22.8~228.0mg.L-1(r=0.999 9),平均加样回收率为99.56%,RSD为1.38%;脱水穿心莲内酯的线性范围为10.7~107.1mg.L-1(r=0.999 9),平均加样回收率为101.41%,RSD为1.70%。结论:该方法简便,结果准确,可用于该制剂的质量控制。     

高效液相色谱法测定消炎止咳片中穿心莲内酯和脱水穿心莲内酯的含量

［摘要］目的建立高效液相色谱（HPLC）法测定消炎止咳片中穿心莲内酯和脱水穿心莲内酯含量。方法采用(Agilent)ZORBAX XDB C18（4.6 mm×150 mm，5 μm）色谱柱，检测波长250nm，流动相：甲醇 水（55：45）流速：1.0 mL·min-1柱温：25 ℃。结果穿心莲内酯线性范围为14.5～145.0 μg·mL 1（r＝0.999 8）；脱水穿心莲内酯线性范围为11.7～117.0 μg·mL 1（r＝0.999 9），穿心莲内酯平均回收率为98.8%，脱水穿心莲内酯平均回收率为99.4%。结论该方法分离效果好、精密度高、准确性好，可以作为消炎止咳片中穿心莲内酯和脱水穿心莲内酯含量测定的方法。     

HPLC法测定穿心莲注射液中脱水穿心莲内酯的含量

目的:建立HPLC法测定穿心莲注射液中脱水穿心莲内酯的含量。方法:色谱柱:Hypersil ODS2 C_(18)柱(250mm×4.6mm,5μm);流动相:甲醇-水(55:45);流速1.0ml·min~(-1),检测波长250nm。结果:脱水穿心莲内酯在0.18～0.90μg的范围内,与峰面积呈良好的线性关系(r=1.000 0)。回收率为99.5%,RSD=2.0%。结论:本法快速、准确、简便。     

双波长HPLC法同时测定穿心莲浸膏中穿心莲内酯和脱水穿心莲内酯的含量

目的建立双波长高效液相色谱法同时检测穿心莲浸膏中穿心莲内酯和脱水穿心莲内酯的含量测定方法。方法采用Intersil C18色谱柱（250 mm×4.6 mm,5μm）,以甲醇—水（60∶40）为流动相;检测波长穿心莲内酯为225 nm,脱水穿心莲内酯为254 nm;柱温为35℃;流速为1.0 mL·min-1。结果穿心莲内酯进样量在0.1043～1.0430μg范围内与峰面积呈良好的线性关系（r=1.000 0,n=5）,脱水穿心莲内酯进样量在0.099 9～0.999 0μg范围内与峰面积呈良好的线性关系（r=1.000 0,n=5）;穿心莲内酯的平均加样回收率为98.53%（RSD=1.27%,n=6）,脱水穿心莲内酯的平均加样回收率为101.51%（RSD=1.10%,n=6）。结论该方法灵敏度高,重现性好,能准确测定穿心莲浸膏中穿心莲内酯和脱水穿心莲内酯的含量。     

Cardenolide analogues. 2. 22-Methylenecard-14-enolides.

22-Methylene-3beta-hydroxy-5beta,20(S)-card-14-enolide (11) and 22-methylene-3beta-hydroxy-5beta,20(R)-card-14-enolide (12) were synthesized from digitoxin (1). Attempts to prepare the 14beta-hydroxy-22-methylene analogues were unsuccessful. The 20(R) isomer (12) was found in Na+, K+-ATPase inhibition studies to be twice as active as 14-dehydrogitoxigenin (17). The 20(S) isomer (11) was significantly less active than 17. The hydrolysis of steroid 3beta-tert-butyldimethysilyl ethers was also found to be much more difficult than with nonsteroids.     

Sila-Pharmaka, 20. Mitt. Sila-Analogon des Tiemoniumiodids

Sila-Drugs, XX: Sila-Analogue of Tiemonium Iodide Silatiemonium iodide (16b) , a sila-analogue of the anticholinergic tiemonium iodide (16a) , and the sila-analogue 14b of the corresponding free base 14a were synthesized for the first time. Compounds 14b and 16b as well as their precursors 10–13 and 15 were characterized by their physical and chemical properties. Their structures were confirmed by elementary analyses, ¹H NMR and mass spectroscopy. The spasmolytic properties of the pairs 14a/14b and 16a/16b were compared on the isolated guinea pig ileum.     

OF4949, new inhibitors of aminopeptidase B. III. Biosynthesis

To elevate production of OF4949 by Penicillium rugulosum OF4949 and to elucidate the pathway of its biosynthesis, mutants were selected on the basis of their resistance to growth inhibition by phenylalanine analogs. A mutant resistant to m-fluorophenylalanine, strain No. M414, had 3-fold the production of the parent. In a study of the biosynthesis of OF4949-I and II, several 14C-labeled compounds were examined as possible precursors of OF4949. L-[14C]Tyrosine and L-[14C]asparagine were incorporated efficiently. Most of the radioactivity of L-[14C]tyrosine was found in the 4-methylisodityrosine (B2) or isodityrosine (B1) moieties, and that of L-[14C]asparagine was in the beta-hydroxyasparagine moiety.     

Studies on the biosynthesis of the antibiotic streptozotocin (streptozocin) by Streptomyces achromogenes var. streptozoticus. Feeding experiments with carbon-14 and tritium labelled precursors.

Feeding experiments and chemical degradations have shown that D-[1(-14)C,2(-3)H]-and-[1(-14)C,6(-3)H] glucosamine, L-[ureido-14C] citrulline, L-[guanidino-14C] arginine and L-[14CH3] methionine specifically label the glucosamine moiety, the urea carbonyl and the N-methyl group of the antibiotic streptozotocin, respectively. Feeding these precursors in amounts of 5 approximately 10 mumoles per 100 ml of culture medium under conditions where the fermentation yielded approximately 20 mumoles of streptozotocin in 24 hours gave incorporation rates which approached 40%. Upon feeding 100 mumoles of either D-[1(-14)C] glucosamine or L-[ureido-14C] citrulline they were incorporated into newly synthesized streptozotocin essentially without dilution by endogeneous precursors. D-[1(-14)C, 6(-3)H] Glucosamine was incorporated without change in T/C ratio while 20% of the tritium was lost from D-[1(-14)C,2(-3)H] glucosamine, suggesting the possibility that D-glucosamine can partially equilibrate with D-fructose prior to its incorporation.     

Metabolism of anethole. I. Pathways of metabolism in the rat and mouse

The metabolic fate of the naturally occurring food flavouring trans-anethole has been investigated in rats and mice. A single 50-mg/kg dose of trans-[methoxy-14C]anethole was given orally to female Wistar albino rats and by ip injection to male CD-1 mice. The major routes of elimination of 14C were the urine and expired air (as 14CO2). Excretion of 14C in the faeces and as volatile compounds in the expired air was very low (total less than 2% of the dose). Urinary metabolites were separated by solvent extraction, TLC and HPLC and were characterized by MS and GC-MS directly and following methylation or trimethylsilylation, the results being compared where possible with authentic standards. Eleven 14C-containing urinary metabolites were identified in the rat and ten in the mouse. These compounds arose from side-chain oxidation, side-chain cleavage and various conjugations. The major urinary metabolites were two isomers of 1-(4'-methoxyphenyl)propane-1,2-diol, 2-hydroxy-1-methylthio-1-(4'-methoxyphenyl)propane and 4-methoxyhippuric acid, the first three all being excreted as glucuronides. In addition to these 14C-labelled metabolites, 4-hydroxypropenylbenzene, the unlabelled product of oxidative O-demethylation of trans-[14C]anethole, was excreted extensively in urine as the glucuronide.     

Synthesis of 14C-labeled optically active N-methyl-barbiturates. 14. Barbituric acid derivatives

Synthesis of ¹⁴C-Labelled Optically Active N-Methylbarbiturates Syntheses of methylurea-[¹⁴CO] and of the hexobarbital and methylcyclobarbital antipodes, ¹⁴C-labelled on C-2 of the heterocyclic nucleus, in the mmole-scale are described.     

螺旋链霉菌一个菌株14^#的特性

用孟外光诱导螺旋链霉菌的溶源化菌株，得到一个不释放噬菌体的品系。这个品系。１４＾＃对温和噬菌体Ｐ１１还有免疫性。瑟慎吸印一分子杂交的结果表明菌株１４＾＃染色体ＤＮＡ和温和噬菌体Ｐ１１的ＤＮＡ有同源性。推测菌株１４＾＃可能是一个缺陷溶源性菌株。     

The [14C]-aminopyrine breath test. A comparison of different forms of analysis.

1 Following ingestion of [14C]-aminopyrine, breath 14CO2 data were analysed from normal individuals, patients with hepatic disease, epileptics receiving anticonvulsant therapy and volunteers before and after treatment with glutethimide. 2 The 'standard' 2 h [14C]-aminopyrine breath test discriminated successfully between the main groups but failed to detect the change in microsomal enzyme function produced by glutethimide. 3 A 'modified' form of the 2 h breath test calculated from the area under the breath specific activity curve detected the increase in demethylation following glutethimide. 4 The breath elimination constant (Kb) derived from the breath 14CO2 disappearance curve was as sensitive as the 'modified' 2 h breath test and was simpler to compute. 5 Glutethimide 500 mg/day for 14 days resulted in a 42% increase in the metabolic clearance of antipyrine and a 26% increase in demethylation of [14C]-aminopyrine.     

A new series of natural antifungals that inhibit P450 lanosterol C-14 demethylase. II. Mode of action.

From a Penicillium sp. we identified a new series of antifungals having a tetrahydropyran skeleton with an alkenyl side chain. We elucidated the mode of action of Ro 09-1470, the most active compound of the series. Treatment of Candida albicans with the compound caused an accumulation of C-14 methyl intermediates of ergosterol at concentrations of which no significant interference with the biosyntheses of other macromolecules and respiration was observed. P450 lanosterol C-14 demethylase (P450(14DM)) activity was inhibited and furthermore, the binding of Ro 09-1470 to the heme of the enzyme was demonstrated by a difference spectrum. We conclude that Ro 09-1470 is the first natural antifungal that inhibits the P450(14DM) of fungi.