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1.
摘 要 目的:建立HPLC ELSD同时测定咳灵胶囊中的苦杏仁苷、桃叶珊瑚苷、哈帕苷、贝母辛、贝母素甲和贝母素乙含量的方法。 方法: 采用Ultimate XB C18色谱柱(250 mm×4.6 mm,5 μm),蒸发光散射检测器(漂移管温度105 ℃,氮气流速2.0 L·min-1);以乙腈 甲醇(1〖KG*9〗∶〖KG-*2〗1)与0.4%醋酸溶液为流动相,进行梯度洗脱,流速:0.7 ml·min-1,柱温:35 ℃。 结果: 苦杏仁苷、桃叶珊瑚苷、哈帕苷、贝母辛、贝母素甲和贝母素乙的线性范围分别为13.56~271.20 μg·ml-1(r=0.999 2)、8.48~169.60 μg·ml-1(r=0.999 9)、4.89~97.80 μg·ml-1(r=0.999 7)、2.66~53.20 μg·ml-1(r=0.999 4)、1.82~36.40 μg·ml-1(r=0.999 8) 、2.04~40.80 μg·ml-1(r=0.999 6);平均加样回收率(RSD)分别为97.90%(1.20%),99.21%(1.62%),97.68%(0.75%),98.36%(1.38%),99.70%(0.79%),97.95%(1.56%)(n=6)。结论: 本文建立的方法结果准确,重复性好,样品处理简便,可作为咳灵胶囊的质量控制方法。 相似文献
2.
摘 要 目的:建立RP HPLC双波长法同时测定参莲胶囊中氧化苦参碱、槐定碱、氧化槐果碱、苦参碱、槐果碱、粉防己碱、防己诺林碱7种生物碱含量。 方法: 采用Venusil XBP NH2(250 mm×4.6 mm,5 μm)色谱柱,以乙腈 0.01%醋酸铵水溶液为流动相梯度洗脱,流速为1.0 ml·min-1,检测波长为210 nm、280 nm。 结果: 氧化苦参碱、槐定碱、氧化槐果碱、苦参碱、槐果碱、粉防己碱、防己诺林碱线性范围分别为32.07~513.07 μg·ml-1(r=0.998 8)、37.90~606.40 μg·ml-1(r=0.999 2)、23.07~369.07 μg·ml-1(r=0.999 2)、52.37~837.87 μg·ml-1(r=0.999 7)、17.63~282.13 μg·ml-1(r=0.999 1)、5.30~84.80 μg·ml-1(r=0.999 5)、8.87~141.87 μg·ml-1(r=0.999 7);平均加样回收率(n=9)为100.16%~102.84%(RSD≤2.0%)。5批样品中氧化苦参碱、槐定碱、氧化槐果碱、苦参碱、槐果碱、粉防己碱、防己诺林碱含量依次为9.18~9.69 mg·g-1、9.35~11.74 mg·g-1、6.73~7.09 mg·g-1、15.17~15.96 mg·g-1、5.03~5.33 mg·g-1、1.23~1.97 mg·g-1、2.48~2.74 mg·g-1。 结论: 所建立的多成分分析方法可用于参莲胶囊中7个生物碱成分的含量测定。 相似文献
3.
摘 要 目的:建立HPLC波长切换法同时测定舒肝益脾液中7个成分。 方法: 色谱柱:Luna C18柱(250 mm×4.6 mm,5 μm);流动相:乙腈 0.05%磷酸溶液,梯度洗脱;流速:0.9 ml·min-1;检测波长:345 nm(滨蒿内酯)、254 nm(毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素)和210 nm(去氢茯苓酸和茯苓酸);柱温:30 ℃,进样量:10 μl。结果: 滨蒿内酯、毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮、芒柄花素、去氢茯苓酸、茯苓酸7个成分的线性范围分别为6.09~152.25 μg·ml-1(r=0.999 9)、2.42~60.50 μg·ml-1(r=0.999 8)、1.61~40.25 μg·ml-1(r=0.999 6)、2.95~73.75 μg·ml-1(r=0.999 4)、6.88~172.00 μg·ml-1(r=0.999 9)、2.55~63.75 μg·ml-1(r=0.999 5)、2.09~52.25 μg·ml-1(r=0.999 9);平均加样回收率分别为98.96%(RSD=1.18%),97.89%(RSD=1.41%),97.18%(RSD=0.88%),96.87%(RSD=0.97%),99.32%(RSD=1.25%),96.77%(RSD=0.86%)和98.55%(RSD=1.03%)(n=9)。结论: 本文建立的HPLC波长切换法同时测定舒肝益脾液中的7个成分,方法简便,可作为舒肝益脾液全面可靠的质量控制方法。 相似文献
4.
张小龙孙晓姚晨旭陈洪岩吴启南 《中国药师》2018,(3):518-520
摘 要 目的:建立同时测定肚痛丸中6种成分含量的气相色谱方法。方法: 色谱柱为 HP 5柱 (30 m×0.32 mm,0.25 μm);采取程序升温,载气为氮气,流速为2.0 ml·min-1,进样量为1 μl,分流比为5∶1,进样口温度为280 ℃,检测器(FID)温度为300 ℃。结果:桂皮醛、乙酸龙脑酯、木香烃内酯、去氢木香内酯、厚朴酚、和厚朴酚分别在32.28~516.40 μg·ml-1(r=0.999 3)、27.06~433.00 μg·ml-1(r=0.999 2)、25.65~410.40 μg·ml-1(r=0.999 3)、26.10~417.60 μg·ml-1(r=0.999 3)、24.01~384.20 μg·ml-1(r=0.999 0)、18.32~293.10 μg·ml-1(r=0.999 4)范围内呈良好的线性关系;平均加样回收率分别为99.71%(RSD=0.67%)、99.34%(RSD=1.18%)、100.16%(RSD=0.34%)、100.40%(RSD=0.39%)、99.32%(RSD=1.22%)、99.58%(RSD=0.58%)(n=6)。结论:该方法操作简便,灵敏度高,准确度好,可为控制该制剂的质量提供依据。 相似文献
5.
摘 要 目的:建立HPLC法同时测定复方羚角降压片中8种活性成分的含量。 方法: 采用HPLC波长切换法,色谱柱为Agilent ZORBAX Eclipse XDB C18(250 mm×4.6 mm,5 μm),流动相为甲醇(A) 0.06%磷酸溶液(B),梯度洗脱,流速为1.0 ml·min-1,检测波长为265 nm(紫丁香苷)、330 nm(咖啡酸、异迷迭香酸苷、迷迭香酸)、278 nm(黄芩苷、汉黄芩苷、黄芩素、汉黄芩素),柱温为30℃,进样量为10 μl。 结果: 紫丁香苷、咖啡酸、异迷迭香酸苷、迷迭香酸、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素分别在11.616~69.696 μg·ml-1,1.601~9.605 μg·ml-1,2.040~12.240 μg·ml-1,14.888~89.328 μg·ml-1,72.032~432.192 μg·ml-1,24.016~144.096 μg·ml-1,10.040~60.240 μg·ml-1,1.801~10.805 μg·ml-1(r为0.999 4~0.999 9)浓度范围内呈良好的线性关系;平均加样回收率分别为98.8%,99.7%,98.8%,98.0%,99.1%,99.3%,100.2%,97.4%,RSD分别为0.7%,0.7%,0.4%,0.6%,0.3%,0.5%,0.5%,0.7%(n=6)。 结论: 该方法简单、有效、准确,可用于复方羚角降压片中上述8种活性成分含量的同时测定。 相似文献
6.
摘 要 目的:建立一测多评法测定黄芪 柴胡药对中8种成分含量。 方法: 采用HPLC法,以黄芪皂苷Ⅰ为内标物,分别计算其与毛蕊异黄酮葡萄糖苷、芒柄花苷、黄芪甲苷、黄芪皂苷Ⅲ、柴胡皂苷c、柴胡皂苷a和柴胡皂苷d的相对校正因子(RCF),通过RCF计算黄芪 柴胡药对中上述7种成分的含量(计算值),同时采用外标法测定上述8种成分的含量(实测值),比较计算值与实测值的差异。色谱柱为Waters sunfire C18(250 mm×4.6 mm,5 μm)柱,流动相为乙腈 0.3%甲酸溶液梯度洗脱液,流速为0.8 ml·min-1,检测器为蒸发光散射检测器,柱温为30℃,进样量为10 μl。 结果: 毛蕊异黄酮葡萄糖苷、芒柄花苷、黄芪甲苷、黄芪皂苷 Ⅲ、黄芪皂苷Ⅰ、柴胡皂苷c、柴胡皂苷a和柴胡皂苷d的线性范围分别为13.680~191.500 μg·ml-1、2.478~34.690 μg·ml-1、2.042~28.590 μg·ml-1、7.278~101.900 μg·ml-1、16.880~236.300 μg·ml-1、2.506~35.080 μg·ml-1、10.260~143.700 μg·ml-1、19.760~276.700 μg·ml-1(r分别为0.999 7,0.999 5,0.999 3,0.999 6,0.999 7,0.999 4,0.999 5,0.999 6);平均加样回收率分别为98.2%,98.8%,98.9%,99.1%,98.7%,99.0%,98.5%,98.2%(RSD均<1.6%)。毛蕊异黄酮葡萄糖苷、芒柄花苷、黄芪甲苷、黄芪皂苷Ⅲ、柴胡皂苷c、柴胡皂苷a和柴胡皂苷d的RCF分别为1.037,0.759,1.247,0.995,1.085,0.587,0.635,其计算值和实测值之间差异无统计学意义(P>0.05)。 结论: 该方法简单、有效、结果准确、节约成本,可用于黄芪 柴胡药对中上述8种活性成分的同时测定。 相似文献
7.
摘 要 目的:建立高效液相色谱法同时测定化瘀祛斑胶囊中芍药苷、黄芩苷和黄芩素的含量。方法: 色谱柱为Agilent Zorbax SB C18柱(150 mm×4.6 mm,5 μm);流动相为甲醇 0.1%磷酸溶液,梯度洗脱;流速为1.0 ml·min-1;检测波长为230 nm(0~15 min),277 nm(15~45 min);柱温为25℃;进样量为10 μl。结果: 芍药苷、黄芩苷和黄芩素的线性范围分别为1.295~25.890 μg·ml-1(r=0.999 9)、30.050~601.000 μg·ml-1(r=0.999 9)、1.874~37.480 μg·ml-1(r=0.999 9),平均回收率分别为100.9%,100.3%,99.31%,RSD分别为0.92%,1.30%,0.89%。结论: 该法简便、快捷、结果准确、重复性好、实用性强,可以用于化瘀祛斑胶囊的质量控制。 相似文献
8.
摘 要 目的:建立HPLC法测定鼻炎愈合剂中阿魏酸、绿原酸和蒙花苷含量。方法: 以Agilent ZORBAX SB C18柱(250 mm×4.6 mm,5 μm)为色谱柱,流动相为乙腈 0.1%磷酸溶液,梯度洗脱,流速为1.0 ml·min-1,柱温30℃,检测波长326 nm。结果: 绿原酸、阿魏酸、蒙花苷分别在3.039 7~30.396 8 μg·ml-1 (r=0.999 7),3.999 9~39.999 4 μg·ml-1 (r=0.999 9),5.820 7~58.207 2 μg·ml-1(r=0.999 9)范围内与峰面积呈良好线性关系,其平均加样回收率分别为98.92%,100.81%,99.89%,RSD分别为1.00%,1.02%,0.99%(n=6)。结论: 该方法操作简便、准确、重现性好,可用于鼻炎愈合剂的质量控制。 相似文献
9.
摘 要 目的:建立HPLC CAD法测定硫酸卡那霉素注射液中卡那霉素和卡那霉素B含量的方法。方法: 采用Boston Green ODS C18(250 mm×4.6 mm,5 μm)色谱柱,以0.2 mol·L-1三氟醋酸溶液 甲醇(95 ∶〖KG-*2〗5)作为流动相,流速:1.0 ml·min-1,柱温:30℃,喷雾温度:55℃,喷雾压力:56.4 psi。结果:卡那霉素在0.385~38.500 μg·ml-1之间呈现良好的线性关系(r=0.999 9),检出限为0.075μg·ml-1,定量限为0.154 μg·ml-1,回收率为100.97%(n=9)。卡那霉素B在0.374~37.400 μg·ml-1之间呈现良好的线性关系(r=1.000 0),检出限为0.075 μg·ml-1,定量限为0.150 μg·ml-1,回收率为100.44%(n=9)。结论:建立的HPLC CAD测定卡那霉素和卡那霉素B含量的方法检出限低,操作简单准确,可以有效控制硫酸卡那霉素注射液的质量。 相似文献
10.
摘 要 目的:建立HPLC波长切换法同时测定参茸固本片中7个成分含量的方法。 方法: 采用Waters Sunfire C18(250 mm×4.6 mm,5 μm)色谱柱,柱温30 ℃,以乙腈 0.1%磷酸溶液为流动相,梯度洗脱,流速为0.9 ml·min-1, 检测波长分别为330 nm(毛蕊花糖苷、马替诺皂苷)、230 nm(芍药内酯苷、芍药苷)和203 nm(人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1)。 结果:毛蕊花糖苷、马替诺皂苷、芍药内酯苷、芍药苷、人参皂苷Rg1、人参皂苷Re和人参皂苷Rb1 质量浓度分别在6.38~159.50 μg·ml-1(r=0.999 3)、3.19~79.75 μg·ml-1(r=0.999 9)、4.37~109.25 μg·ml-1(r=0.999 5)、14.26~356.50 μg·ml-1(r=0.999 4)、1.95~48.75 μg·ml-1(r=0.999 8)、2.21~55.25 μg·ml-1(r=0.999 7)、2.09~52.25 μg·ml-1(r=0.999 1)范围内与峰面积线性关系良好;平均加样回收率(RSD)分别为98.24%(1.11%)、97.64%(1.43%)、99.23%(0.80%)、100.13%(0.65%)、96.99%(1.56%)、98.10%(1.24%)和97.75%(1.37%)。结论:本文所建立的方法实现了同时测定参茸固本片中毛蕊花糖苷、马替诺皂苷、芍药内酯苷、芍药苷、人参皂苷Rg1、人参皂苷Re和人参皂苷Rb1的含量,可用于参茸固本片的质量控制。 相似文献
11.
Boobis AR 《Environmental toxicology and pharmacology》1996,2(2-3):161-163
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
12.
M. ASHTON 《Xenobiotica; the fate of foreign compounds in biological systems》2013,43(2):195-204
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
13.
Markus Müller Bettina v.Osten Rainer Schmid Evelyne Piegler Ingeborg Gerngroß 《Naunyn-Schmiedeberg's archives of pharmacology》1995,352(4):438-441
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
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.
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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18.
Allegaert K de Hoon J Verbesselt R Devlieger H Tibboel D 《European journal of clinical pharmacology》2005,60(12):911-913
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
19.
Alana Upthagrove Jin Chen Charles D. Meyers Kenneth Kulmatycki Angela Bretz Lai Wang 《Xenobiotica; the fate of foreign compounds in biological systems》2017,47(12):1077-1089
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
20.
Changes in immunoreactive somatostatin in brain following lidocaine-induced kindling in rat 总被引:3,自引:0,他引:3
The kindling phenomenon has become a useful model for studying epileptogenesis. The present authors have previously reported increased levels of immunoreactive somatostatin (IR-SRIF) in various regions of the brain of electrically-amygdaloid kindled (EAK) rats. In this study, an examination was made of immunoreactive somatostatin in pharmacologically-kindled (PK) rats. Sixteen male Sprague-Dawley rats were injected intraperitoneally (i.p.) with a subthreshold dose of lidocaine (60 mg/kg), once daily. Once the kindling phenomenon was established, kindled rats (7), non-kindled rats (9) and controls (6) were sacrificed by microwave irradiation. Another group of 5 rats was injected with a single suprathreshold dose of lidocaine (110 mg/kg) and killed 10 min after the resultant seizure. Various brain areas were removed and assayed for immunoreactive somatostatin in kindled rats. Immunoreactive somatostatin was significantly greater than in controls in the amygdala (56%; P less than 0.02), entorhinal + piriform cortex (50%; P less than 0.05) and hypothalamus (29%; P less than 0.02). In non-kindled rats, immunoreactive somatostatin increased only in the amygdala (58%; P less than 0.02). No difference was found in the immunoreactive somatostatin content of rats injected with an suprathreshold dose of lidocaine compared to controls. The alteration of immunoreactive somatostatin, in both lidocaine-kindled and electrically-amygdaloid kindled rats suggests a possible role of this neuropeptide in kindling. 相似文献