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1.
目的 建立同时测定消疲灵颗粒中7种成分含量的HPLC波长切换联合梯度洗脱方法。方法 采用Venusil MP-C18色谱柱,流动相为乙腈-1%冰醋酸溶液,流速为0.9 mL·min-1,梯度洗脱,柱温为30 ℃,进样量为10 μL。结果 牡荆素葡萄糖苷、牡荆素鼠李糖苷、牡荆素、金丝桃苷、芒柄花苷、毛蕊异黄酮和芒柄花素检测浓度分别在2.56~51.20 μg·mL-1,14.87~297.40 μg·mL-1,2.14~42.80 μg·mL-1,3.16~63.20 μg·mL-1,3.80~76.00 μg·mL-1,2.14~42.80 μg·mL-1,4.81~ 96.20 μg·mL-1内与峰面积呈良好的线性关系(r≥0.999 1),平均回收率97.0%~100.0%,RSD 0.55%~1.67%,精密度和重复性良好,供试品溶液在室温条件下12 h内稳定。结论 该方法操作简便,精密度、稳定性、重复性好,可用于消疲灵颗粒中7种有效成分含量的同时测定。  相似文献   

2.
目的 采用LC-MS/MS测定人血浆中乙酰左卡尼汀的浓度并用于氯乙酰左卡尼汀片在健康受试者体内的药动学研究。方法 健康受试者单次给药0.5,1.0,1.5 g和多次给予0.5 g后,0~24 h采集血样。通过测定单次和多次给药后血浆中乙酰左卡尼汀的绝对浓度,计算其药动学参数。米屈肼为内标,经甲醇沉淀蛋白后进行LC-MS/MS分析。ESI离子源正离子模式监测,检测离子m/z 204.3→145.2(乙酰左卡尼汀),m/z 147.2→58.2(米屈肼);色谱柱为EC 250/4.6 NUCLEOSIL100-5CN,流动相为甲醇-10 mmol·L-1乙酸铵溶液(含0.1%甲酸)(85:15)。结果 乙酰左卡尼汀在20~3 000 μg·L-1内线性良好(r=0.999 1),最低定量限为20 μg·L-1。批内、批间精密度及基质效应RSD均<15%。单次给药3个剂量组(0.5,1.0,1.5 g)的主要药动学参数为:AUC0-t为(4 181.77±2 473.24)μg·h·L-1、(6 099.54±1 939.41)μg·h·L-1和(8 064.71±3 575.99)μg·h·L-1Cmax为(611.42±270.76)μg·L-1,(830.92±233.19)μg·L-1和(1 004.67±414.95)μg·L-1t1/2z为(4.50±2.93)h、(6.25±3.65)h和(5.76±3.94)h;多次给药后主要的药动学参数:AUC0-t为(13 728.82±6 493.04)μg·h·L-1Cmax为(1 129.00±374.05)μg·L-1t1/2z为(8.57±4.42)h。结论 本方法准确、灵敏、专属性强,适用于人体内乙酰左卡尼汀药动学研究。单次和多次给予氯乙酰左卡尼汀片后药动学参数有明显差异,性别间无差异,健康受试者对药物的耐受性良好。  相似文献   

3.
目的 建立LC-MS/MS同时测定大鼠血浆中5种银杏酸的浓度,并进行药动学研究。方法 大鼠血浆样品用乙酸乙酯萃取后,以水杨酸为内标,选用ZORBAX Eclipse XDB C18(2.1 mm×100 mm,3.5 μm)色谱柱,以乙腈-水(均含0.1%甲酸)为流动相梯度洗脱,梯度流速恒定为0.25 mL·min-1,柱温为30℃,进样量为10 μL,总分析时间为5.0 min,采用电喷雾离子化源,负离子方式,多反应监测(MRM)扫描方式进行监测。结果 血浆中5种银杏酸浓度线性范围为2.0~1 000 μg·L-1r>0.99),定量下限为2.0 μg·L-1;质控样品准确度为92.8%~108.5%;日内、日间RSD均<15%;提取回收率为73.3%~86.2%。结论 该方法快速、灵敏、准确,专属性强,重复性好,适用于同时测定大鼠血浆中5种银杏酸浓度。  相似文献   

4.
目的 建立一种高灵敏度HPLC测定大鼠血浆中益母草碱浓度,并研究益母草碱在大鼠体内的药动学特征。方法 大鼠口服益母草碱混悬溶液(50 mg·kg-1)后,不同时间点尾静脉采血,以苯甲酰精氨酸乙酯为内标,血浆样品经酸化后乙酸乙酯萃取,采用HPLC进行测定。色谱条件:采用Diamonsil C18(250 mm×4.6 mm,5 μm)为色谱柱,以乙腈-0.02 mol·L-1磷酸二氢钾缓冲溶液(pH 3.0)(22:78)为流动相,流速1.0 mL·min-1,柱温35℃,检测波长277 nm。并利用PKS 1.0软件计算药动学参数。结果 益母草碱血浆浓度在0.05~1.5 μg·mL-1内线性关系良好(r=0.999 1)。方法的定量下限(LLOQ)为0.05 μg·mL-1(RSD=12.8%,n=5);提取回收率为76.5%~82.5%;批内、批间准确度为96.9%~104.9%;日内、日间精密度均<10%;质控样品经反复冻融3次及-20℃放置1个月后均较稳定。大鼠口服益母草碱后,药-时曲线符合二室开放模型,主要药动学参数为tmax=0.95 h,Cmax=0.51 μg·mL-1t1/2=3.64 h,AUC0-t=1.56 μg·mL-1·h-1,AUC0-∞=1.78 μg·mL-1·h-1结论 该方法准确度、灵敏度高,重复性好,可用于生物样品中益母草碱浓度的测定。  相似文献   

5.
目的 建立UPLC测定中成药和保健食品中16种非法添加的抗过敏类药物。方法 采用Waters BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),以甲醇-20 mmol·L-1磷酸二氢钠(用磷酸调节pH值至3.0)为流动相,梯度洗脱,检测波长为220 nm。结果 16种抗过敏类药物在2.5~40 μg·mL-1内呈良好线性关系(r2>0.999),平均回收率为90.77%~113.35%,RSD为0.06%~1.21%;定量限为0.18~3.92 μg·mL-1,检出限为0.09~0.78 μg·mL-1结论 该方法简便、灵敏度高,可有效地判断中成药及保健品中是否非法掺入16种抗过敏类药物。  相似文献   

6.
目的 建立HPLC测定人工关节假体周围感染患者关节液中万古霉素浓度的方法。方法 以替硝唑为内标,采用Hypersil C18柱(250 mm×4.6 mm,5 μm),流动相为乙腈-0.012 5mol·L-1磷酸二氢钾缓冲液(pH=3.2)(10:90),流速1 mL·min-1,柱温35℃,检测波长236 nm,进样量10 μL。结果 关节液中万古霉素浓度在0.906 8~90.681 8 μg·mL-1线性良好。批内、批间精密度RSD均<15%,准确度85.89%~103.51%。结论 本法易于操作,精密度和准确度良好,适用于人工关节假体周围感染患者关节液中的万古霉素浓度监测。  相似文献   

7.
头孢克洛分散片中聚合物测定   总被引:1,自引:1,他引:0  
目的 建立2种头孢克洛聚合物有效的测定方法并对结果进行比较。方法 方法1:采用TSKgel G2000SWxl色谱柱(7.8 mm×300 mm,5 μm),流动相为0.01 mol·L-1磷酸盐缓冲液[0.01 mol·L-1 NaH2PO4溶液-0.01 mol·L-1 Na2HPO4溶液(50︰50),调节pH值为7.0]-乙腈(95︰5),流速为0.5 mL·min-1柱温35℃,检测波长为254 nm,进样量20 μL;方法2:采用Sephadex G-10色谱柱(10 mm×300 mm,40~120 μm),以0.05 mol·L-1磷酸盐缓冲液[取0.05 mol·L-1 Na2HPO4溶液-0.05 mol·L-1 NaH2PO4溶液(50︰50),调节pH至7.0]为流动相A,水为流动相B,流速为1 mL·min-1,柱温35℃,检测波长为254 nm,进样量100 μL。结果 方法1:头孢克洛主峰与聚合物峰分离度>1.5,头孢克洛质量浓度在0.25~20 μg·mL-1内线性关系良好(r=0.999 9);定量限0.21 μg,检测限0.07 μg。重复性较好(RSD为1.8%,n=6);在拟定的色谱条件下,通过考察破坏坏性实验(高温、强酸、强碱、氧化、光照)能够满足分离度要求,辅料无干扰;方法2:质量浓度在2.5~20 μg·mL-1线性关系良好(r=0.999 7);检测限0.13 μg,定量限0.40 μg。重复性良好(RSD为1.8%,n=6)。结论 新建立的2种方法对于头孢克洛分散片聚合物的分离度好,分离效率高,重复性好,均可以作为头孢克洛分散片的质量控制的依据。  相似文献   

8.
HPLC同时测定消炎利胆片中5种活性成分的含量   总被引:1,自引:1,他引:0  
目的 建立HPLC同时测定消炎利胆片中5种活性成分(绿原酸、迷迭香酸、穿心莲内酯、芹菜素、脱水穿心莲内酯)的方法。方法 采用phenomonex®-C18色谱柱(4.6 mm×250 mm,5 μm),以乙腈(A)-0.4%的磷酸水溶液(B)为流动相进行梯度洗脱,流速为1.0 mL·min-1,柱温为30℃,检测波长为330 nm(绿原酸、迷迭香酸、芹菜素)和254 nm(穿心莲内酯、脱水穿心莲内酯)。结果 绿原酸、迷迭香酸、穿心莲内酯、芹菜素和脱水穿心莲内酯检测浓度分别在3.042~121.7 μg·mL-1、2.558~102.3 μg·mL-1、14.11~564.4 μg·mL-1、2.835~113.4 μg·mL-1、23.86~954.3 μg·mL-1内与峰面积呈良好的线性关系(r ≥ 0.999 6),平均加样回收率为97.90%~101.75%,RSD为0.89%~1.66%,仪器精密度、重复性、稳定性良好。结论 本试验所建立的方法准确可靠、重复性好,可为消炎利胆片的质量控制提供科学的依据。  相似文献   

9.
目的 建立GC-MS/MS测定中药材中18种多氯联苯(PCBs)的方法。方法 采用超声提取,浓硫酸净化,内标法定量;采用EI源,在多反应监测(MRM)模式下进行检测。结果 18种PCBs在0.5~50 ng·L-1时线性关系良好,相关系数(r)为0.999 8~1.000 0,方法的检出限为0.013~0.080 μg·kg-1,定量限为0.054~0.328 μg·kg-1。在2,5,10 μg·L-1下平均回收率分别为106.7%~118.7%,93.5%~114.7%和89.9%~115.6%,相对标准偏差分别为1.6%~8.0%,2.7%~4.6%和1.0%~3.1%。结论 本方法样品处理简单、快速,灵敏度高,准确性好,可用于中药材中18种PCBs的测定。  相似文献   

10.
目的 建立HPLC波长切换法同时测定心神安胶囊中9种成分的含量。方法 采用Agilent Eclipse XDB-C18色谱柱,流动相乙腈(A)-0.1%甲酸溶液(B),梯度洗脱;流速0.9 mL·min-1;检测波长分别为320 nm[检测远志(口山)酮Ⅲ、3,6''-二芥子酰基蔗糖]、203 nm (检测人参皂苷Rb1、绞股蓝皂苷XLIX、绞股蓝皂苷XVⅡ)和254 nm (检测毛蕊异黄酮葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素);柱温25℃。结果 远志(口山)酮Ⅲ、3,6''-二芥子酰基蔗糖、人参皂苷Rb1、绞股蓝皂苷XLIX、绞股蓝皂苷XVⅡ、毛蕊异黄酮葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素分别在2.070~41.40 μg·mL-1r=0.999 2)、3.860~77.20 μg·mL-1r=0.999 6)、11.29~225.8 μg·mL-1r=0.999 8)、5.070~101.4 μg·mL-1r=0.999 9)、19.86~397.2 μg·mL-1r=0.999 5)、1.280~25.60 μg·mL-1r=0.999 1)、0.960 0~19.20 μg·mL-1r=0.999 3)、0.670 0~13.40 μg·mL-1r=0.999 7)、2.580~51.60 μg·mL-1r=0.999 1)内线性关系良好,平均回收率分别为98.04%,99.26%,99.05%,97.42%,100.0%,98.27%,97.81%,96.84%和99.86%,RSD分别为1.28%,0.82%,1.43%,1.43%,0.86%,1.26%,1.38%,1.16%和0.69%。结论 本方法操作简便、准确、重复性好,能够对心神安胶囊中9种成分进行同时含量测定,为提高和完善心神安胶囊的质量标准提供了有效方法。  相似文献   

11.
Several biochemical and cellular effects have been described for methylxanthines under in vitro conditions. However, it is unknown, whether threshold concentrations required to exert these effects are attained in target tissues in vivo. We therefore employed the microdialysis technique for measuring theophylline concentrations in peripheral tissues under in vivo conditions.Following in vitro and in vivo calibration, microdialysis probes were inserted into the medial vastus muscle and into the periumbilical subcutaneous adipose layer of healthy volunteers. Following single oral dose administration of 300 mg or i.v. infusion of 240 mg theophylline, in vivo time courses of theophylline concentrations were monitored in tissues and plasma. Major pharmacokinetic parameters (cmax, tmax, AUC) were calculated for plasma and tissue time courses. The mean AUCtissue /AUCplasma-ratio was 0.56 (p.o.) and 0.55 (i.v.) for muscle and 0.55 (p.o.) and 0.72 (i.v.) for subcutaneous adipose tissue.We conclude that microdialysis provides important information on the distribution and the tissue pharmacokinetics of theophylline.Abbreviations FPIA Fluorescence polarisation immuno assay - AUC Area under the curve - tmax Time to peak concentration - cmax Peak concentration  相似文献   

12.
In assessing interindividual variability in metabolic activation, the toxic metabolite is often too unstable for conventional analysis. Possible alternatives include a stable product of the reactive metabolite e.g. cysteinyl derivatives of N-acetyl-4-benzoquinoneimine, the toxic metabolite of paracetamol, adducts with DNA or protein, and indirect measurement of the activity of the enzyme(s) producing the active metabolite. An example of the last approach is the use of furafylline, a highly specific inhibitor of human CYP1A2, to determine the extent of the metabolic activation of the cooked food mutagens PhIP and MeIQx. The extent of inhibition, determined from levels of unchanged amine in urine, is an indirect measure of the activity of the activation pathway. Further refinement of this approach, allied to improved measures of the biological process of interest should prove of value in evaluating interindividual variability and its role in the risk assessment process.  相似文献   

13.
1. The pharmacokinetics of the antimalarial compound artemisinin were compared in the male and female Sprague-Dawley rat after single dose i.v. (20 mg.kg) or i.p. (50 mg.kg) administration of an emulsion formulation. 2. Plasma clearance of artemisinin was 12.0 (95% confidence interval: 10.4, 13.0) l.h. kg in the male rat and 10.6 (95% CI: 7.5, 15.0) l.h. kg in the female rat suggesting high hepatic extraction in combination with erythrocyte uptake or clearance. Artemisinin half-life was 0.5 h after both routes of administration in both sexes. Values for plasma clearance and half-lives did not statistically differ between the sexes. 3. After i.p. administration artemisinin AUCs were 2-fold higher in the female compared with male rat (p 0.001). Artemisinin disappearance was 3.9-fold greater in microsomes from male compared with female livers and it was inhibited in male microsomes by goat or rabbit serum containing antibodies against CYP2C11 and CYP3A2 but not CYP2B1 or CYP2E1. 4. The unbound fraction of artemisinin in plasma was lower (p 0.001) in plasma obtained from the male (8.8 2.0%) compared with the female rat (11.7 2.2%). 5. The possibility of a marked sex difference, dependent on the route of administration, has to be taken into account in the design and interpretation of toxicological studies of artemisinin in this species.  相似文献   

14.
本实验测定10名休克患者血浆和红细胞的丙二醛(MDA)、血浆总抗的氧化活性(AOA)的含量。结果表明:休克病人红细胞膜和血浆 MDA 含量(4.298±0.722;5.348±0.834)与对照组(3.235±0.682;4.356±1.081)比较明显增高(P<0.05);血浆 AOA(39.65±7.858)与对照组(48.21±10.81)比较明显降低(P<0.01)。提示:休克时,患者机体内自由基反应增强是引起组织细胞损伤的原因之一。  相似文献   

15.
Polymorphisms in genes involved in neurotransmission in relation to smoking   总被引:4,自引:0,他引:4  
Smoking behavior is influenced by both genetic and environmental factors. The genetic contribution to smoking behavior is at least as great as its contribution to alcoholism. Much progress has been achieved in genomic research related to cigarette-smoking within recent years. Linkage studies indicate that there are several loci linked to smoking, and candidate genes that are related to neurotransmission have been examined. Possible associated genes include cytochrome P450 subfamily polypeptide 6 (CYP2A6), dopamine D1, D2, and D4 receptors, dopamine transporter, and serotonin transporter genes. There are other important candidate genes but studies evaluating the link with smoking have not been reported. These include genes encoding the dopamine D3 and D5 receptors, serotonin receptors, tyrosine hydroxylase, trytophan 2,3-dioxygenase, opioid receptors, and cannabinoid receptors. Since smoking-related factors are extremely complex, studies of diverse populations and of many aspects of smoking behavior including initiation, maintenance, cessation, relapse, and influence of environmental factors are needed to identify smoking-associated genes. We now review genetic polymorphisms reported to be involved in neurotransmission in relation to smoking.  相似文献   

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1.?Pradigastat is a potent and specific diacylglycerol acyltransferase-1 (DGAT1) inhibitor effective in lowering postprandial triglycerides (TG) in healthy human subjects and fasting TG in familial chylomicronemia syndrome (FCS) patients.

2.?Here we present the results of human oral absorption, metabolism and excretion (AME), intravenous pharmacokinetic (PK), and in vitro studies which together provide an overall understanding of the disposition of pradigastat in humans.

3.?In human in vitro systems, pradigastat is metabolized slowly to a stable acyl glucuronide (M18.4), catalyzed mainly by UDP-glucuronosyltransferases (UGT) 1A1, UGT1A3 and UGT2B7. M18.4 was observed at very low levels in human plasma.

4.?In the human AME study, pradigastat was recovered in the feces as parent drug, confounding the assessment of pradigastat absorption and the important routes of elimination. However, considering pradigastat exposure after oral and intravenous dosing, this data suggests that pradigastat was completely bioavailable in the radiolabeled AME study and therefore completely absorbed.

5.?Pradigastat is eliminated very slowly into the feces, presumably via the bile. Renal excretion is negligible. Oxidative metabolism is minimal. The extent to which pradigastat is eliminated via metabolism to M18.4 could not be established from these studies due to the inherent instability of glucuronides in the gastrointestinal tract.  相似文献   

19.
Diclofop-methyl (DM) is a chlorophenoxy derivative used in large quantities for the control of annual grasses in grain and vegetable crops. In this study, the genotoxic effects of DM were investigated by measuring chromosomal aberrations (CAs) in mouse bone-marrow cells and CA and the comet assay in human peripheral lymphocytes. Mice were treated with 15.63, 31.25, 62.5, and 125?mg/kg body weight of DM intraperitoneally for 24 hours, and 15.63-, 31.25-, 62.5-, 125-, and 250-µg/mL concentrations were applied to human lymphocytes for both 24 and 48 hours. In in vivo treatments, DM significantly, but not dose dependently, increased the total chromosome aberrations, compared to both negative and solvent controls. Cell proliferation was significantly, but not dose dependently, affected by all doses. In in vitro treatments, DM (except 15.63 µg/mL) significantly and dose dependently increased the frequency of chromosome aberrations. Also, 250 µg/mL of 48-hour treatment was found to be toxic. Cell proliferation was significantly and dose dependently affected by DM applications, when compared to negative control. In in vitro treatments, DM significantly decreased the mitotic index only at the highest concentration for 24 hours, and 62.5- and 125-µg/mL concentrations for 48 hours. In the comet assay, a significant and dose-dependent increase in comet-tail intensity was observed at 62.5-, 125-, and 250-µg/mL concentrations. The mean comet-tail length was significantly increased in all concentrations. Our results demonstrate that DM is genotoxic in mammalian cells in vivo and in vitro.  相似文献   

20.
Based on blood and cerebrospinal fluid samples collected in a full-term neonate, the penetration of tramadol in the central nervous system is described. Following intravenous administration of tramadol, a lag time of about 4 h was observed until full blood–brain equilibration was achieved. This pharmacokinetic observation is in line with a recent pharmacodynamic evaluation of the central opioid effects of tramadol in adults.  相似文献   

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