高效液相色谱法同时测定不同产地枳壳药材中柚皮苷、橙皮苷、新橙皮苷、异柚皮苷的含量

目的建立同时测定枳壳药材中柚皮苷、橙皮苷、新橙皮苷、异柚皮苷含量的方法。方法采用高效液相色谱法,色谱柱VenusilXBP C18柱（250 mm×4.6 mm,5μm）,流动相为乙腈-0.1%甲酸（梯度洗脱）,检测波长为283 nm,流速为1 mL/min;柱温为30℃。结果柚皮苷进样量在0.5～5μg范围与峰面积线性关系良好,r=0.999 8;异柚皮苷在0.08～2.01μg范围线性良好,r=0.999 8;橙皮苷在0.06～1.2μg范围线性关系良好,r=0.999 9;新橙皮苷在0.09～4.82μg范围线性关系良好,r=0.999 7。异柚皮苷、柚皮苷、橙皮苷和新橙皮苷平均加样回收率分别为101.17%,98.25%,95.42%和100.95%。结论该方法简便、准确、可靠,适用于枳壳药材质量控制。     

常山胡柚不同生长期果实中3种成分含量的动态变化

目的 建立HPLC同时测定常山胡柚不同生长期果实中柚皮苷、橙皮苷、新橙皮苷含量的方法,并研究常山胡柚不同生长期果实中3种成分含量的动态变化,从而确定常山胡柚作为药用资源的最佳采收时间。方法 采用HPLC测定常山胡柚不同生长期果实中柚皮苷、橙皮苷、新橙皮苷3种成分的含量,色谱柱为安捷伦ZORBAX SB-C₁₈(4.6 mm× 250 mm,5 μm);流动相为乙腈-0.2%磷酸(15∶85);检测波长：284 nm;流速：1.0 mL·min^-1;柱温：40 ℃;峰面积外标法定量。结果 柚皮苷、橙皮苷、新橙皮苷的线性范围分别为28.45~284.50 ng(r=0.999 8)、18.09 ~180.93 ng(r=0.999 8)、85.86~858.55 ng(r=0.999 6),平均回收率分别为98.83%(RSD=2.12%),99.05%(RSD=2.30%),98.83%(RSD=1.85%)。常山胡柚不同生长期果实中柚皮苷、橙皮苷、新橙皮苷的含量分别为12.65~109.66,0.45~17.50,8.06~218.90 mg·g^-1,柚皮苷在6月时最高,橙皮苷和新橙皮苷在5月时最高,其中5~7月间采收的果实柚皮苷和新橙皮苷的含量均符合中国药典枳壳项下含量的要求。结论 本方法操作简便、快速,结果准确、可靠,重复性好,适合作为含量测定的方法,并为常山胡柚作为药用资源的采收提供了参考依据。     

HPLC测定银花芒果片中绿原酸、芒果苷和橙皮苷的含量

目的 建立HPLC同时测定银花芒果片中绿原酸、芒果苷和橙皮苷的含量。方法 采用Waters SunFire^TM C₁₈ (4.6 mm×150 mm,5 μm)色谱柱;流动相为甲醇(A)-0.2%磷酸水溶液(B),梯度洗脱,流速为1.0 mL·min^-1,检测波长为327 nm(0~10 min,绿原酸),258 nm(10~20 min,芒果苷),283 nm(20~40 min,橙皮苷)。结果 绿原酸进样量在0.140~2.516 μg内线性关系良好(r=0.999 9,n=6),平均回收率为99.4%,RSD为1.2%(n=9);芒果苷进样量在0.042~0.761 μg内线性关系良好(r=0.999 9,n=6),平均回收率为99.9%,RSD为1.4%(n=9)。橙皮苷进样量在0.076~1.361 μg内线性关系良好(r=0.999?8,n=6),平均回收率为99.9%,RSD为0.7%(n=9)。结论 该方法简便、快捷、准确,可用于该制剂的质量控制。     

HPLC法测定通舒口爽胶囊中3种成分的含量

目的建立测定通舒口爽胶囊中柚皮苷,橙皮苷和新橙皮苷含量的HPLC方法。方法采用Diamonsil C18(200 mm×4.6 mm,5μm)色谱柱,流动相:甲醇-乙腈-体积分数为0.05%的磷酸水溶液(体积比为20∶10∶65),流速:1.0 mL.min-1,柱温:30℃,检测波长:280 nm。结果柚皮苷在8.88~88.8 mg.L-1内呈线性关系(r=0.999 7),平均回收率为100.5%;橙皮苷在7.60~76.0 mg.L-1内呈线性关系(r=0.999 6),平均回收率为100.5%;新橙皮苷在10.56~105.6 mg.L-1内呈线性关系(r=0.999 9),平均回收率为100.5%。结论本实验建立的方法可作为通舒口爽胶囊质量控制方法之一。     

六味开胃消食颗粒质量标准的建立

摘 要 目的： 建立六味开胃消食颗粒的质量标准。方法: 采用TLC法对六味开胃消食颗粒中的枳壳、木香、白术和山楂等药材进行了薄层色谱鉴别;采用HPLC法测定君药枳壳药材中柚皮苷与新橙皮苷的含量,色谱柱为Sinochrom ODS BP（250 mm×4.6 mm,5 μm）,流动相：乙腈-0.1%磷酸（21∶79）;流速：1.0 ml·min^-1;检测波长：283 nm;柱温：30℃。结果: 薄层色谱法可鉴别出该制剂中的枳壳、木香、白术和山楂。柚皮苷在89.600～1.792×10³ μg范围内有良好的线性关系（r=0.999 8）,新橙皮苷在1.060×10²～2.120×10³ μg范围内有良好的线性关系（r=0.999 9）,柚皮苷平均回收率为98.67%,RSD为0.57%（n=6）,新橙皮苷平均回收率为98.07%,RSD为1.19%（n=6）。结论: 该方法准确、灵敏、重复性好,能有效的控制六味开胃消食颗粒的质量。     

HPLC同时测定衢枳壳中7种指标成分的含量

目的 建立HPLC同时测定衢枳壳中芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、木犀草素、川陈皮素和桔皮素含量。方法 采用Agilent Extend C₁₈（4.6 mm×250 mm,5 μm）色谱柱,检测波长：330 nm,以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速：1 ml·min^-1,柱温：30℃。结果 芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、木犀草素、川陈皮素、桔皮素分别在23.30~1 164.80 ng,170.84~8 541.91 ng,17.22~861.20 ng,156.17~7 808.64 ng,3.13~156.48 ng,0.90~45.23 ng,0.85~42.27 ng内线性关系良好（r ≥ 0.999 5,n=6）,平均回收率分别为98.8%,101.3%,98.3%,96.8%,101.8%,101.7%,108.9%。结论 首次建立了衢枳壳中7个成分HPLC含量测定方法,该方法简便,结果准确,可为综合评价衢枳壳质量提供依据。     

HPLC同时测定橘红枇杷胶囊中橙皮苷、柚皮苷的含量

目的 建立HPLC法测定橘红枇杷胶囊中橙皮苷、柚皮苷含量.方法 液相色谱法.色谱柱为Waters Fire C18柱（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.5%磷酸溶液（19：81）;流速：1.0 mL·min-1;柱温：30℃;检测波长283 nm.结果 橙皮苷进样量在0.236～23.6 μg范围内呈良好线性关系（r=1.000 0,n=8）,平均加样回收率为100.1%,RSD为3.3%（n=9）; 柚皮苷进样量在0.134～13.4 μg范围内呈良好线性关系（r=0.999 2,n=8）,平均加样回收率为105.1%,RSD为3.2%（n=9）.结论 该方法简便快速,结果准确,可作为本品质量控制方法.     

RP-HPLC法测定前列癃闭通片中柚皮苷、新橙皮苷的含量

摘 要 目的: 建立反相高效液相色谱测定前列癃闭通片中柚皮苷、新橙皮苷的含量测定方法。方法: 色谱柱为WEL TECH Hisep C₁₈-T（250 mm×4.6 mm,5 μm）;流动相：乙腈-水（20∶80）（用磷酸调节pH值至3）;流速：1.0 ml·min^-1;检测波长：283 nm;柱温：25℃,进样量：10 μl。结果: 柚皮苷进样量在0.143～3.570 μg内呈良好的线性关系;新橙皮苷进样量在0.164～4.110 μg内呈良好的线性关系。两者的平均回收率分别为99.06%、98.40%,RSD分别为1.64%、1.29%（n=6）。结论: 该检测方法准确、可靠、重现性好,可用于前列癃闭通片中柚皮苷、新橙皮苷的含量测定。     

HPLC法同时测定胃痛丸中柚皮苷、新橙皮苷的含量

摘 要 目的：建立胃痛丸中柚皮苷、新橙皮苷的高效液相色谱法（HPLC）含量测定方法。方法: 采用HPLC,色谱柱为Agilent TC C18 柱 ,以乙腈-水（20∶80）为流动相,流速为1.0ml·min^-1,检测波长为283 nm,柱温为30℃。 结果: 柚皮苷和新橙皮苷分别在0.027～4.552 μg( r=0.999 9) 、0.029～4.016 μg( r=0.999 8) ,进样量与峰面积呈良好的线性关系,平均加样回收率分别为102.19%、103.60%,RSD分别为2.88% 、1.79%( n=9)。 结论:方法简便、准确、灵敏、重复性好,可作为胃痛丸中的柚皮苷和新橙皮苷含量控制方法。     

HPLC测定芩暴红止咳胶囊中东莨菪内酯、黄芩苷、黄芩素和杜鹃素的含量

目的 采用HPLC测定芩暴红止咳胶囊中东莨菪内酯、黄芩苷、黄芩素、杜鹃素的含量。方法 Eclipse XDB-C₁₈色谱柱(4.6 mm×250 mm,5 μm),流动相：甲醇(A)-1%冰醋酸溶液(B),梯度洗脱,流速：0.8 mL·min^-1;检测波长：295 nm;柱温：30 ℃。结果 东莨菪内酯线性范围为1.27~124.70 μg,r=0.999 9,加样回收率为98.3%(RSD=1.1%);黄芩苷线性范围为8.07~538.20 μg,r=1.000 0,样品加样回收率为98.0%(RSD=1.2%);黄芩素线性范围为1.12~111.60 μg,r=1.000 0,加样回收率为98.5%(RSD=0.9%);杜鹃素线性范围为1.06~106.40 μg,r=1.000 0,加样回收率为99.0%(RSD=1.4%)。结论 本方法简便、准确,重复性好,专属性高,可用于制剂的质量控制。     

Affective and Anxiety Disorders and Alcohol and Drug Dependence:

Depression and anxiety frequently coexist in patients with substance use disorders. This clinically-oriented article examiens the relationship between these conditions and emphasizes data showing that substances of abuse can cause signs and symptoms of both depression and anxiety. These substance-related syndromes appear to have a different course and prognosis than uncomplicated, independent anxiety and major depressive disorders, and clinicians should consider the role of alcohol and other drugs in all patients presenting with these complaints. The authors will also outline an approach for diagnosing and managing patients with the combination of a substance use and depressive or anxiety disorder.     

Modelling and simulation of variability and uncertainty in toxicokinetics and pharmacokinetics

Two important methodological issues within the framework of the variability and uncertainty analysis of toxicokinetic and pharmacokinetic systems are discussed: (i) modelling and simulation of the existing physiologic variability in a population; and (ii) modelling and simulation of variability and uncertainty when there is insufficient or not well defined (e.g. small sample, semiquantitative, qualitative and vague) information available. Physiologically based pharmacokinetic models are especially suited for separating and characterising the physiologic variability from the overall variability and uncertainty in the system. Monte Carlo sampling should draw from multivariate distributions, which reflect all levels of existing dependencies in the intact organism. The population characteristics should be taken into account. A fuzzy simulation approach is proposed to model variability and uncertainty when there is semiquantitative, qualitative and vague information about the model parameters and their statistical distributions cannot be defined reliably.     

Antiinfective and encrustation-inhibiting materials--myth and facts

Catheters, urethral and ureteral stents and other urological implants are frequently affected by encrustration and infection due to their permanent contact with urine. Indwelling urinary catheters provide a haven for microorganisms and thus require extensive monitoring. Several surface modification techniques have been proposed to improve the performance of devices including the immobilization of biomolecules, the incorporation of hydrophilic grafts to reduce protein adsorption, the creation of hydrophobic surfaces, the creation of microdomains to regulate cellular and protein adhesion, new polymers and antimicrobial coatings. Physico-chemical explanation to elucidate the mechanism of such encrustation or infection inhibiting materials is still not available. Our series of experiments showed a marked decrease of silver-activity in biological fluids which corresponds with the controversial clinical results obtained with silver coated urinary catheters. Rifampicin/minocycline coated catheters had very low activity against Gram-negative rods, enterococci and Candida spp., the main causing organisms of urinary catheter infection. Surface engineered materials and antimicrobial drug delivery systems will be the next generation of sophisticated urinary catheters and stents, if both efficacy as well as efficiency has been proved clinically.     

Synthesis and anti-nociceptive and anti-inflammatory effects of gaultherin and its analogs

The synthesis of gaultherin (1) and its analogs was carried out to provide 11 glycosides under phase-transfer catalytic conditions. The activities of all synthesized compounds were evaluated by nitric oxide production inhibitory assay in vitro. Methyl 2-O-(4-O-β-d-galactopyranosyl)-β-d-glucopyranosylbenzoate (5f) showed significantly anti-nociceptive and anti-inflammatory effects by the evaluation in vivo. Structure–activity relationships within these compounds were discussed.     

Interaction of estrone and estradiol with DNA and protein of liver and kidney in rat and hamster in vivo and in vitro

[6,7-³H] Estrone (E) and [6,7-³H]estradiol-17 (E₂) have been synthesized by reduction of 6-dehydroestrone and 6-dehydroestradiol with tritium gas. Tritiated E and E₂ were administered by oral gavage to female rats and to male and female hamsters on a dose level of about 300 g/kg (54 mCi/kg). After 8 h, the liver was excised from the rats; liver and kidneys were taken from the hamsters. DNA was purified either directly from an organ homogenate or via chromatin. The radioactivity in the DNA was expressed in the units of the Covalent Binding Index, CBI = (mol chemical bound per mol DNA-P)/(mmol chemical administered per kg b.w.). Rat liver DNA isolated via chromatin exhibited the very low values of 0.08 and 0.09 for E and E₂, respectively. The respective figures in hamster liver were 0.08 and 0.11 in females and 0.21 and 0.18 in the males. DNA isolated from the kidney revealed a detectable radioactivity only in the female, with values of 0.03 and 0.05 for E and E₂, respectively. The values for male hamster kidney were < 0.01 for both hormones. The minute radioactivity detectable in the DNA samples does not represent covalent binding to DNA, however, as indicated by two sets of control experiments. (A) Analysis by HPLC of the nucleosides prepared by enzyme digest of liver DNA isolated directly or via chromatin did not reveal any consistent peak which could have been attributed to a nucleoside-steroid adduct. (B) All DNA radioactivity could be due to protein contaminations, because the specific activity of chromatin protein was determined to be more than 3,000 times higher than of DNA. The high affinity of the hormone to protein was also demonstrated by in vitro incubations, where it could be shown that the specific activity of DNA and protein was essentially proportional to the concentration of radiolabelled hormone in the organ homogenate, regardless of whether the animal was treated or whether the hormone was added in vitro to the homogenate.Carcinogens acting by covalent DNA binding can be classified according to potency on the basis of the Covalent Binding Index. Values of 10³–10⁴ have been found for potent, 10² for moderate, and 1–10 for weak carcinogens. Since estrone is moderately carcinogenic for the kidney of the male hamster, a CBI of about 100 would be expected. The actually measured limit of detection of 0.01 places covalent DNA binding among the highly unlikely mechanisms of action. Similar considerations can be made for the liver where any true covalent DNA binding must be below a level of 0.01. It is concluded that an observable tumor induction by estrone or estradiol is unlikely to be due to DNA binding.Paper presented at the Satellite Symposium of the European Society of Toxicology, Rome, March 29, 1983     

成骨细胞的功能与损伤和骨质疏松的防治

骨质疏松是一种全身性骨骼疾病,导致骨折风险增加。成人的骨量通过破骨细胞的骨吸收和成骨细胞的骨形成作用来维持动态平衡,治疗骨质疏松症的理想策略是抑制破骨细胞的骨吸收和/或增强成骨细胞的骨形成功能。目前针对保护成骨细胞及增强其功能的骨质疏松疗法相对较少。因此,本文针对成骨细胞相关功能蛋白、各种细胞损伤机制（内质网应激、氧化应激、机械过载、微小RNA和长链非编码RNA的影响等）及骨质疏松的治疗与预防作一综述,以期为针对增强成骨细胞功能的骨质疏松治疗策略提供新思路。     

益生菌与肿瘤防治

益生菌广泛存在于自然界中,通过维持宿主体内菌群平衡、影响肠屏障功能和调节免疫应答等作用,提高宿主健康水平,被公认为"肠道健康卫士".一些益生菌可以增强机体的免疫功能,抑制致癌物质,影响肿瘤细胞的基因表达,对肿瘤具有拮抗作用.大量研究表明,益生菌在未来的肿瘤防治中有很好的应用和发展前景.     

Isolation and characterization of glycosylated and non-glycosylated prolactins from alligator and crocodile

Two molecular forms of prolactin (PRL). glycosylated and non-glycosylated, were isolated from pituitary glands of two reptiles, alligator and crocodile. The reptilian PRLs were extracted under alkaline conditions from the precipitate obtained after pituitaries were first extracted with 0.25 m sucrose, 1 mM NH₄HCO₃, pH 6.3. Purification was performed by ion exchange chromatography on DE-52, gel filtration on Sephadex G-75 superfine, and reversed phase high performance liquid chromatography. Two forms of both alligator and crocodile PRL, designated PRLI and PRLII, with molecular weights of 26000 and 24000 were isolated. Alligator and crocodile PRLI and PRLII were stained specifically in immunoblots with anti-sea turtle PRL and anti-ostrich PRL. Sequence analysis revealed that both forms of alligator and crocodile PRLs consisted of 199 amino acid residues with a glycosylation consensus sequence (Asn-Ala-Ser) at position 60 in alligator and crocodile PRLs with a molecular weight of 26000 (PRLI). In contrast, Thr was substituted for Asn at position 60 in the PRLs with a molecular weight of 24000 (PRLII). The sequences of alligator PRLs differed from crocodile PRLs only in position 134: Val for alligator PRLs and He for crocodile PRLs. There is a high degree of structural conservation between the reptilian PRLs isolated in this study and avian PRL; each showed 92% sequence identity with chicken PRL and 89% with turkey PRL.     

Pharmacokinetics and pharmacodynamics of ramipril and piretanide administered alone and in combination

The pharmacokinetics and pharmacodynamics of single oral doses of 5 mg ramipril and 6 mg piretanide administered separately and in combination were determined in a single blind, randomised, 3-period cross-over study in 24 healthy male volunteers.The peak plasma concentrations of ramipril and ramiprilat increased slightly (from 11.9 to 14.8 ng/ml, and from 6.39 to 8.96 ng/ml, respectively) as did the area under the plasma concentration-time curve of ramipril (0–4 h) and ramiprilat (0–24 h) (from 15.8 to 19.8 ng·ml^–1·h, and from 63.4 to 74.6 ng·ml^–1·h, respectively). The urinary excretion of ramiprilat also rose (from 6.82 to 7.73 % of dose) following simultaneous treatment with piretanide. These effects were probably due to reduced first-pass metabolism of ramipril/ramiprilat to inactive metabolites. The blood pressure lowering effect, the time course of inhibition of ACE activity in plasma and the concentration-response relationship for the inhibition of plasma ACE activity were not affected by piretanide.The peak plasma concentration of piretanide was somewhat reduced (from 285 to 244 ng/ml) following simultaneous treatment with ramipril. No other pharmacokinetic parameter was affected. Piretanide increased urine flow, and sodium, chloride and potassium excretion, especially during the first 2 hours following administration. These pharmacodynamic parameters were not affected by ramipril.Thus, simultaneous administration of single oral doses of ramipril and piretanide caused modest changes in the peak and average plasma concentrations of both drugs, which did not lead to detectable alterations in the pharmacodynamic parameters measured in healthy volunteers.