34种吴茱萸中吴茱萸碱和吴茱萸次碱的含量测定

建立了吴茱萸中吴茱萸碱和吴茱萸次碱的反相高效液相色谱法 ,并用该法测定了 34种不同产地及不同炮制方法吴茱萸中吴茱萸碱和吴茱萸次碱的含量 .采用峰面积内标法定量 .吴茱萸碱和吴茱萸次碱在 0 5～ 2 0g/mL范围内均呈线性 ,相关系数分别为 0 9999、0 9998,平均回收率分别为 96 6 %、96 0 %     

超临界流体萃取吴茱萸中吴茱萸碱和吴茱萸次碱

目的研究超临界流体萃取(SFE)吴茱萸中吴茱萸碱和吴茱萸次碱的提取工艺,并用高效液相色谱法(HPLC)测定吴茱萸碱和吴茱萸次碱的含量.方法采用95%乙醇作夹带剂,运用超临界流体的萃取工艺,含量测定时,在Water-C18柱上,以乙腈-水(43∶57)为流动相,流速1.0 mL*min-1,检测波长290 nm,柱温40℃.结果吴茱萸碱和吴茱萸次碱的标准曲线在0.024～0.120 μg(r=0.9994)和0.026～0.130 μg(r=0.9995)之间有较好的线性关系;加样平均回收率分别为102.7%(RSD=1.58)和101.7%(RSD=1.79%). 结论采用SFE萃取吴茱萸中吴茱萸碱和吴茱萸次碱的提取工艺速度快,HPLC法测定吴茱萸碱和吴茱萸次碱的含量精确,重现性好.     

HPLC方法测定华佗再造丸中阿魏酸、吴茱萸内酯、吴茱萸碱和吴茱萸内碱的研究

目的 建立HPLC法测定华佗再造丸中阿魏酸、吴茱萸内酯、吴茱萸碱及吴茱萸次碱的含量.方法 采用Waters SunFire C18（4.6mm×250mm,5μm）色谱柱,以乙腈-0.1%磷酸进行梯度洗脱,流速1.0mL·min-1,阿魏酸检测波长为323nm,吴茱萸内酯、吴茱萸碱检测波长为225nm,吴茱萸次碱检测波长为343nm,柱温30℃.结果 表明阿魏酸、吴茱萸内酯、吴茱萸碱和吴茱萸次碱分别在3.91～39.10μg·mL-1（r=1.0000）、10.70～64.20μg·mL-1（r=0.9998）、7.60～76.00μg·mL-1（r=0.9999）、3.65～36.50μg·mL-1（r=0.9999）范围内与峰面积呈良好的线性关系;平均回收率（n=6）分别为96.6%（RSD=1.0%）、98.1%（RSD=2.2%）、100.3%（RSD=0.8%）、95.3%（RSD=1.2%）.结论 本文方法简便准确,可用于华佗再造丸中阿魏酸、吴茱萸内酯、吴茱萸碱及吴茱萸次碱的含量测定.     

HPLC法测定超微戊己丸中吴茱萸碱和吴茱萸次碱含量

目的：建立超微戊己丸中吴茱萸碱和吴茱萸次碱的含量测定方法。方法采用Kromasail C18色谱柱（250mm×4.6mm,5μm）,流动相为流速1.0mL/min的乙腈-乙腈10%（50：50）,测定波长为225nm。结果吴茱萸碱和吴茱萸次碱理论板数分别为2681和2067,Y吴茱萸碱=1.965×10^-7X ＋0.07646,r=0.9999）, Y吴茱萸次碱=3.658×10^-7X-0.2199,r=0.9999）,吴茱萸碱与吴茱萸次碱的线性区间分别为10.2～51.0μg/mL以及10.0～50.0μg/mL ,两者平均回收率分别为97.3%和101.4%,其相对标准偏差分别为3.2%和3.9%,最低检测限为0.05μg/mL和0.1μg/mL。结论使用高效液相色谱法对超微戊己丸当中的吴茱萸碱以及吴茱萸次碱含量进行检测的精确率较高,重现性好。     

吴茱萸不同炮制品中吴茱萸碱、吴茱萸次碱、柠檬苦素含量测定

目的:考察不同炮制方法及炮制前后吴茱萸中吴茱萸碱、吴茱萸次碱和柠檬苦素的含量变化情况。方法:采用高效液相色谱法,Hypersil ODS C₁₈（250 mm×4.6 mm,5μm）;流动相:乙腈-水-四氢呋喃-乙酸（41:59:1:0.2）;流速:1.0 ml·min^-1;检测波长:225 nm;柱温:25℃。结果:吴茱萸碱、吴茱萸次碱、柠檬苦素进样量分别在0.156～3.120μg（r=0.999 6,n=6）、0.116～2.320μg（r=1.000 0,n=6）、0.620～12.400μg（r=0.999 1,n=6）范围内与峰面积呈良好线性关系,平均回收率分别为97.2%（RSD=1.33%）、97.1%（RSD=1.56%）、97.3%（RSD=1.52%）。结论:不同炮制方法吴茱萸碱、吴茱萸次碱、柠檬苦素含量不同,砂烫法优于其他炮制方法。     

不同生产工艺的戊己丸中吴茱萸碱和吴茱萸次碱含质量比较

目的:建立戊己丸中吴茱萸碱和吴茱萸次碱含质量的高效液相(HPLC)测定方法,并对超微戊己丸和常规戊己丸中吴茱萸碱和吴茱萸次碱的含质量进行比较。方法:采用色谱柱HypersilC18柱(4.6mm×250mm,5μm),流动相:乙腈水(48∶52),流速:1mL/min,检测波长:225nm。结果:吴茱萸碱和吴茱萸次碱的理论塔板数均大于3000,吴茱萸碱回归方程:A吴茱萸碱=107.73ρ-14.331,r=0.9999,线性范围1.02～20.4μg/mL;吴茱萸次碱回归方程:A吴茱萸次碱=15.596ρ-45.09,r=0.9998,线性范围4.4～176μg/mL。超微戊己丸中吴茱萸碱平均回收率为:99.61%,RSD为0.50%,质量分数为(0.096±0.0148)%;吴茱萸次碱平均回收率为94.85%,RSD为1.00%,质量分数为(0.343±0.0467)%。常规戊己丸中吴茱萸碱平均回收率为98.56%,RSD为1.70%,质量分数为(0.81±0.003)%;吴茱萸次碱平均回收率为99.55%,RSD为0.50%,质量分数为(0.161±0.0075)%。结论:超微戊己丸中吴茱萸碱和吴茱萸次碱的质量分数高于常规戊己丸。     

HPLC法同时测定吴茱萸中吴茱萸碱、吴茱萸次碱与吴茱萸内酯的含量

目的:建立同时测定吴茱萸中吴茱萸碱、吴茱萸次碱与吴茱萸内酯含量的方法。方法:采用高效液相色谱法。色谱柱为迪马C1(8200mm×4.6mm,5μm),流动相为乙腈-0.04%庚烷磺酸钠溶液(48:52,V/V),流速为1.0mL·min-1,检测波长为225nm,柱温为35℃。结果:吴茱萸碱、吴茱萸次碱、吴茱萸内酯的进样浓度分别在5.38～53.80、5.02～50.20、10.30～103.00μg·mL-(1r均为0.9999)范围内与各自峰面积积分值呈良好线性关系;三者平均加样回收率分别为99.75%、97.66%、85.68%,RSD分别为0.67%、1.16%、1.54%(n=6)。结论:本方法简便、可行、重复性好,可用于吴茱萸中吴茱萸碱和吴茱萸次碱的含量测定;但吴茱萸内酯的回收率较低,需进一步改进其测定方法。     

液质联用法测定吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱在大鼠脑脊液和脑组织中的分布

吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱是吴茱萸中主要的生物碱类成分.为研究吴茱萸主要生物碱成分在大鼠脑脊液中的代谢和在脑组织中的分布,吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱以1∶1∶1的质量比混合,以15 mg/kg的剂量灌胃给予大鼠.本文建立了同时测定大鼠脑脊液和脑组织中三个生物碱成分的液质联用方法,测定结果显示,三个生物碱...     

高效液相色谱法测定吴茱萸药材及其制剂中吴茱萸碱和吴茱萸次碱…

报道了用高效相色谱法测定了吴茱萸汤颗粒剂及吴茱萸药材中吴茱萸碱和吴茱萸冰碱的含量，采用ＯＤＳ柱，以乙腈一水（４３：５７）流动相，于２９０ｎｍ处检测。吴茱萸汤颗粒剂吴茱萸碱和吴茱萸次碱的回收率分别为１０１．５％，９７．０％，ＲＳＤ分别为１．２４％，２．１３％。     

HPLC法测定吴茱萸超微速溶饮片中吴茱萸碱、吴茱萸次碱及柠檬苦素的含量

目的建立一种同步测定吴茱萸超微速溶饮片中吴茱萸碱,吴茱萸次碱及柠檬苦素含量的高效液相色谱方法。方法采用Hypersil ODS2C18柱(4.6mm×250mm,5μm),岛津LC-20AD高效液相色谱仪,流动相为乙腈-水-四氢呋喃-冰醋酸(34:64.7:1.1:0.2),流速:1.0mL/min,检测波长:225nm,柱温:30℃。结果吴茱萸碱、吴茱萸次碱、柠檬苦素进样量分别在0.1016～2.032μg(r2=0.9999,n=6)、0.0974～1.948μg(r2=0.9999,n=6)、0.7010～14.02μg(r2=0.9999,n=6)范围内与峰面积呈良好线性关系,平均回收率分别为100.37%(RSD=1.29%,n=6)、99.11%(RSD=0.83%,n=6)、99.30%(RSD=0.52%,n=6)。结论该测定方法简便,测定结果准确,重复性好,可作为质量控制方法。     

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。     

Comparison of formation of thiolactones and active metabolites of prasugrel and clopidogrel in rats and dogs

1. Prasugrel and clopidogrel are antiplatelet prodrugs that are converted to their respective active metabolites through thiolactone intermediates. Prasugrel is rapidly hydrolysed by esterases to its thiolactone intermediate, while clopidogrel is oxidized by cytochrome P450 (CYP) isoforms to its thiolactone. The conversion of both thiolactones to the active metabolites is CYP mediated. This study compared the efficiency, in vivo, of the formation of prasugrel and clopidogrel thiolactones and their active metabolites.

2. The areas under the plasma concentration versus time curve (AUC) of the thiolactone intermediates in the portal vein plasma after an oral dose of prasugrel (1 mg kg^?1) and clopidogrel (0.77 mg kg^?1) were 15.8 ± 15.9 ng h ml^?1 and 0.113 ± 0.226 ng h ml^?1, respectively, in rats, and 454 ± 104 ng h ml^?1 and 23.3 ± 4.3 ng h ml^?1, respectively, in dogs, indicating efficient hydrolysis of prasugrel and little metabolism of clopidogrel to their thiolactones in the intestine.

3. The relative bioavailability of the active metabolites of prasugrel and clopidogrel calculated by the ratio of active metabolite AUC (prodrug oral administration/active metabolite intravenous administration) were 25% and 7%, respectively, in rats, and 25% and 10%, respectively, in dogs.

4. Single intraduodenal administration of prasugrel showed complete conversion of prasugrel, resulting in high concentrations of the thiolactone and active metabolite of prasugrel in rat portal vein plasma, which demonstrates that these products are generated in the intestine during the absorption process.

5. In conclusion, the extent of in vivo formation of the thiolactone and the active metabolite of prasugrel was greater than for clopidogrel’s thiolactone and active metabolite.

     

PTEN和DNA含量与非小细胞肺癌侵袭转移的关系探讨

目的 研究非小细胞肺癌(NSCLC)组织中抑癌基因PTEN的表达和DNA含量与NSCLC侵袭、转移的关系.方法 采用免疫组织化学SP方法检测PTEN在78例肺癌标本中的表达,并用流式细胞术检测30例肺癌标本中DNA含量.结果:肺癌标本中PTEN蛋白总缺失率为42.3%,有淋巴结转移组和无淋巴结转移组肺癌表达缺失率分别为52.1%和26.7%(P＜0.05),其表达缺失率随TNM分期增加而上升,分期越晚表达缺失率越高.PTEN缺失率高者生存时间短.DNA指数(DI)的分布范围在1.04～1.93.异倍体肿瘤24例,DI值随TNM分期增加而增加(P＜0.05),与淋巴结转移呈正相关.结论 肺癌组织中PTEN的表达与肺癌淋巴结转移有显著相关性,肺癌细胞DNA含量与肺癌TNM分期及淋巴结转移密切相关.检测PTEN蛋白表达和DNA含量将有助于判断肺癌的转移及预后.     

阿立哌唑与利培酮治疗自闭症谱系障碍与注意缺陷多动障碍共病患儿的疗效与安全性评价

目的：评价阿立哌唑与利培酮治疗自闭症谱系障碍（ASD）与注意缺陷多动障碍（ADHD）共病患儿的疗效与安全性。方法：选取在某院精神科治疗的ASD和ADHD共病患儿68例,根据随机数字表法将患儿分为阿立哌唑组（n=34）和利培酮组（n=34）。阿立哌唑组患儿接受起始剂量为5 mg·d^-1的阿立哌唑片口服治疗,最终剂量增加至15 mg·d^-1。利培酮组患儿接受起始剂量为1 mg·d^-1的利培酮片口服治疗,最终剂量增加至2 mg·d^-1;2组患儿均治疗12周。在基线（T₀）、治疗6周（T₁）与12周（T₂）时,采用注意缺陷/多动评定量表（ADHD-RS）评价患儿总体ADHD症状变化情况;采用康纳斯行为评定量表（CRSR）教师用量表多动因子（CRSR-I）评价患儿多动症的改善情况;采用CRSR不注意缺陷-冲动因子（CRSR-H）评价患儿注意力缺陷的改善情况;采用临床整体印象-严重程度量表（CGI-S）及儿童总体评估量表（C-GAS）评分评价患儿整体功能。对患儿的相关临床指标进行常规监测,比较2组患儿药物不良事件与安全性。结果：与T₀时比较,阿立哌唑组患儿T₁与T₂时,ADHD-RS、CRSR-I、CRSR-H与CGI-S评分均显著降低（均P<0.05）,C-GAS评分显著提高（P<0.05）。利培酮组患儿T₂时,ADHD-RS、CRSR-I、CRSR-H与CGI-S评分均显著降低（均P<0.05）,C-GAS评分显著提高（P<0.05）。2组患儿的ADHD症状显著改善,多动症状与不注意缺陷-冲动症状显著改善,患儿的整体功能也显著改善。2组患儿主要的不良事件是食欲增加、体质量增加与嗜睡,但均没有发生严重的不良事件。T₂时,利培酮组患儿催乳素水平显著提高（t=9.619,P<0.001）,其他临床指标没有显著性差异（均P>0.05）。结论：阿立哌唑和利培酮能够通过减少ASD和ADHD共病患儿的注意力涣散和多动症症状来改善患儿整体功能,具有较高的疗效、安全性,值得临床推广应用。     

阿立哌唑与利培酮治疗痴呆精神行为症状的疗效及安全性比较

目的观察阿立哌唑和利培酮治疗老年痴呆精神行为症状的疗效及安全性。方法采用随机对照研究,将具有精神行为症状的痴呆患者68例完全随机分为阿立哌唑组及利培酮组,各34例。阿立哌唑组患者服用阿立哌唑,起始剂量2．5mg／d,最大剂量不超过15mg／d;利培酮组患者口服利培酮,起始剂量0．5mg／d,最大剂量不超过3mg／d。疗程均为8周。治疗前和治疗第2、4、8周末采用痴呆病理分析评定量表（BEHAVE—AD）评定疗效,用副反应量表（TESS）评定不良反应,并于入组时和治疗第8周末分别检测2组患者空腹血糖、餐后2h血糖、TC、TG、LDL—C、HDL—C及体重。结果阿立哌唑组和利培酮组患者治疗2、4、8周后BEHAVE—AD评分均明显低于治疗前[阿立哌唑组：（14．8±4．2）、（10．2±3．6）、（6．8±2．8）分比（16．4±4．6）分;利培酮组：（15．2±3．9）、（11．8±3．8）、（7．2±3．0）分比（17．2±5．O）分,P〈0．05或P〈0．01]。2组患者间治疗前及治疗后BEHAVE—AD评分比较,差异均无统计学意义（P〉0．05）。2组不良反应发生率均为8．8％（3／34）,差异无统计学意义（P〉0．05）。利培酮组治疗8周末体重较治疗前增加明显[（71±6）kg比（66±6）kg,P〈0．05],TG及LDL—C升高[分别为（1．62±0．46）mmol／L比（0．96±0．29）mmol／L．（3．82±0．86）mmol／L比（3．08±0．74）mmol／L,而阿立哌唑组则改变不明显（均P〉0．05）。结论阿立哌唑治疗老年痴呆精神行为症状总体疗效、安全性与利培酮相当,但阿立哌唑对患者血糖、血脂及体重影响小于利培酮。     

Correlation of behavioral and neurochemical effects of d- and l-amphetamines

In an attempt to correlate the behavioral and neurochemical effects of d- and l-amphetamines, the time courses of the effects of the two isomers (1 mg/kg; base, i.p.) were studied on spontaneous motor activity (SMA) and stereotyped behavior (ST) as well as on the concentrations of norepinephrine (NE), dopamine (DA), and serotonin (5-HT) in discrete brain areas, such as the caudate nucleus (CN), pons-medulla (PM), and diencephalonmidbrain (DM) in rats. In addition, the dose-response relationship for d-isomer (0.5–2 mg/kg, i.p.) and l-isomer (1–4 mg/kg, i.p.) was also studied on SMA and ST. SMA increased with the dose up to 1.5 mg/kg for d-isomer and up to 3 mg/kg for l-isomer and then decreased, whereas ST increased with the dose for both the isomers. At 1 mg/kg dose, SMA reached its peak during the fourth postdrug 20–minute period for both d- and l-isomers, whereas ST reached its peak during third to fifth 20-minute periods for d-isomer and during the third period for the l-isomer. The d-isomer significantly increased the DA levels in the CN and DM at 30 minutes postdrug, which reached their maximum at 60 minutes, whereas NE levels in the PM had no significant change at 30 minutes, but were significantly reduced in the DM at 30 minutes and in both PM and DM at 60 minutes postdrug; 5-HT levels in the PM and DM showed no significant change. Compared to d-amphetamine, the l-isomer at 30 and 60 minutes postdrug caused more or less similar changes in the NE levels in the DM and PM, whereas it produced less increase in the DA levels in the CN and DM and significant decrease in 5-HT levels in the DM and PM. It appears that the difference in the behavioral effects induced by the two isomers of amphetamine may be due to the difference in their effects on dopaminergic and serotonergic systems.     

Quantification and prediction of skin pharmacokinetics of amoxicillin and cefuroxime

The purpose of this project was to develop and validate a pharmacokinetic model and to quantify the rate and extent of distribution between plasma and skin of two β‐lactam antibiotics, amoxicillin (AMX) and cefuroxime (CFX), which are frequently administered systemically to treat skin and skin structure infections. Dosing regimens are usually based on plasma concentration, however, concentrations at the target site are better correlated with the effect. For each antibiotic, three different i.v. bolus doses were administered to three female rabbits according to a randomized cross‐over design and plasma samples were collected serially. Skin concentrations were obtained by continuous microdialysis. Skin and unbound plasma concentrations were fitted simultaneously using a semi‐physiological model and the transfer constants plasma/skin (K_in) and skin/plasma (K_out) were estimated. K_in and K_out were then used to predict skin concentrations from the plasma levels obtained from an oral administration of AMX or from an i.v. bolus of CFX. The predicted skin profiles were similar to those measured by microdialysis during the actual experiments. In conclusion, this study shows that it is possible to generate a reasonable prediction of skin pharmacokinetics from any plasma level once a careful characterization of the transfer process between plasma and skin has been made. Copyright © 2009 John Wiley & Sons, Ltd.     

乙肝两对半、前S1抗原与HBV-DNA含量的测定与比较

目的　探讨乙肝两对半、前 S1抗原与 HBV- DNA含量的关系。方法　 183 0份血清用 EL ISA方法测定 HBV“两对半”和前 S1抗原 ,用荧光定量 PCR方法检测 HBV- DNA含量。结果　不同两对半模式血清 HBV-DNA阳性率不同 ,检出率以 HBs Ag( )和 /或 HBe Ag( )组最高 ;共检出前 S1抗原阳性血清 73例 ,其中 HBV-DNA检出率为 90 .4% ( 66/ 73 )。结论　前 S1抗原与 HBe Ag、HBV- DNA有较好相关性 ;FQ- PCR检测可更准确反映 HBV感染及复制情况