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HPLC波长切换联合梯度洗脱法同时测定消疲灵颗粒中的7种成分 总被引:2,自引:2,他引:0
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
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目的 探索新目安眼用即型凝胶相变过程对兔眼内房水中药物药动学特性的影响,并与普通凝胶比较,评价该即型凝胶的剂型特征。方法 以新西兰家兔为试验对象,采用眼部给予新目安眼用即型凝胶(存在相变过程)和普通凝胶后,按时间点取房水,测定更昔洛韦含量,建立药物在房水中的药动学方程,计算体内药动学参数,比较两者的差别。结果 新目安眼用即型凝胶房水中更昔洛韦药动学方程为C=18.94×e-0.015 4 t-18.94×e-0.079 85 t,普通凝胶房水中更昔洛韦药动学方程为C=15.42×e-0.015 3 t-15.42×e-0.048 8 t,说明两者在兔眼内的药动学机制相同。从各药动学参数比较分析,新目安眼用即型凝胶由于相变过程使达峰时间仅为25.51 min,达峰浓度高达10.31 μg·mL-1,吸收半衰期缩短为8.679 min,AUC提高到992.4 μg·mL-1·min,而普通凝胶达峰时间为34.63 min,达峰浓度仅为6.232 μg·mL-1,吸收半衰期为14.20 min,AUC仅为691.4 μg·mL-1·min。结论 即型凝胶相转变过程能将相变潜能(△H)转变成药物角膜渗透的动能,可最大限度发挥药效。 相似文献
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UPLC同时测定中成药和保健食品中16种非法添加的抗过敏类药物 总被引:2,自引:1,他引:1
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
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目的 使用基于鼠伤寒沙门氏菌的Ames波动试验和小鼠淋巴瘤细胞(L5178Y)的体外微核试验评价2种染料金橙Ⅱ和金胺O的遗传毒性风险。方法 在-/+S9处理下,不同质量浓度的金橙Ⅱ和金胺O(0.625~10.000 μg·mL-1)分别与鼠伤寒沙门氏菌组氨酸营养缺陷型菌株TA98和TA100混合后接种于96孔板中,37℃下孵育72 h后判断其对细菌回复突变的影响;在体外微核试验中,在-/+S9处理下,金橙Ⅱ(10~50 μg·mL-1)和金胺O(0.6~1.2 μg·mL-1)分别与L5178Y细胞作用4 h或24 h,并在给药后24 h收集细胞进行流式细胞术检测。结果 金橙II自2.50 μg·mL-1起可引起-S9和+S9处理组的TA98回复性突变孔数显著增加(P<0.05、0.01),代谢活化后增加幅度更为明显;自5 μg·mL-1起可引起-S9处理组的TA100回复性突变孔数显著性增加(P<0.01),作用均呈浓度相关性。10 μg·mL-1金胺O可引起-S9处理组的TA98回复性突变孔数显著增加(P<0.01);自0.625 μg·mL-1起即可引起+S9处理组的TA98回复性突变孔数显著增加(P<0.05、0.01),且存在浓度相关性;自2.5 μg·mL-1起可引起+S9处理组的TA100回复性突变孔数显著性增加(P<0.05、0.01),且存在浓度相关性。在-S9处理组中,30~50 μg·mL-1金橙Ⅱ可引起L5178Y细胞微核率显著增加(P<0.01),且存在浓度相关性; 0.9~1.2 μg·mL-1金胺O可引起L5178Y细胞微核率显著增加(P<0.01),且存在浓度相关性。在+S9处理组中,10~50 μg·mL-1金橙Ⅱ可导致L5178Y细胞微核率显著增加(P<0.05、0.01)。30~50 μg·mL-1金橙Ⅱ可导致S期的L5178Y细胞比例增加;金胺O自0.6 μg·mL-1起即可导致L5178Y细胞亚二倍体细胞核率增加。结论 金橙Ⅱ和金胺O均存在一定的遗传毒性风险。 相似文献
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目的 建立气相色谱-质谱联用法测定碳酸司维拉姆中环氧氯丙烷残留量的方法,以满足原料药质量标准中的限度要求。方法 采用DB-17MS毛细管柱(30 m×0.25 mm,0.25 μm);进样口温度为200℃;离子源温度为230℃;MS四极杆温度为150℃;载气为氦气;柱流量为1.0 mL·min-1;程序升温;分流比为10:1;定量离子m/z 57。结果 在0.087~0.260 μg·mL-1内环氧氯丙烷浓度与峰面积呈现良好的线性关系,定量限为0.045 μg·mL-1,检测限为0.017 μg·mL-1;平均加样回收率为98.4%。结论 该方法简单快速,专属性强,准确度好,灵敏度高,可以满足碳酸司维拉姆原料药标准中的限度要求。 相似文献
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目的 建立UHPLC波长切换法同时测定芎菊上清丸中9种成分的含量方法。方法 采用Agilent Ecilipse C18(2.1 mm×100 mm,1.6 μm)色谱柱,流动相:甲醇-0.05%磷酸水溶液,梯度洗脱;流速为0.3 mL·min-1;检测波长:327,237,320,345,278,254 nm;柱温30℃;进样量2 μL;并采用SPSS 22.0统计软件对含量测定结果进行主成分分析与聚类分析。结果 绿原酸、3,5-二咖啡酰奎宁酸、栀子苷、甘草苷、阿魏酸、盐酸小檗碱、黄芩苷、升麻素苷、5-O-甲基维斯阿米醇苷线性范围分别为4.30~68.80 μg·mL-1(r=0.999 0)、6.66~106.56 μg·mL-1(r=0.999 2)、7.67~122.72 μg·mL-1(r=0.999 4)、4.88~78.08 μg·mL-1(r=0.999 1)、2.37~37.92 μg·mL-1(r=0.999 1)、6.50~103.92 μg·mL-1(r=0.999 2)、8.85~141.60 μg·mL-1(r=0.999 4)、0.88~14.08 μg·mL-1(r=0.999 7)、0.74~11.92 μg·mL-1(r=0.999 3);平均加样回收率(n=9)均在99.42%~103.10%,RSD均<2.0%。主成分分析与聚类分析均可将不同生产厂家的芎菊上清丸很好地分类,且分类结果一致。结论 所建立的多成分方法快捷、准确、重复性好,可用于芎菊上清丸的质量控制。 相似文献
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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
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HPLC同时测定通脉颗粒中丹参素、原儿茶醛、丹酚酸B、阿魏酸和葛根素的含量 总被引:1,自引:1,他引:0
目的 建立通脉颗粒中丹参素、原儿茶醛、丹酚酸B、阿魏酸和葛根素的HPLC测定方法。方法 采用Welch Ultimate XD-C18色谱柱(4.6 mm×250 mm,5 μm),以乙腈-0.1%三氟乙酸为流动相,梯度洗脱,双波长检测(282,305 nm),柱温35℃,流速1.0 mL·min-1。结果 丹参素、丹酚酸B、原儿茶醛、葛根素和阿魏酸的线性范围分别为3.117~62.33 μg·mL-1(r=0.998 7),4.044~80.88 μg·mL-1(r=0.9985),1.280~25.60 μg·mL-1(r=0.997 9),7.964~159.3 μg·mL-1(r=0.992 8),1.980~39.60 μg·mL-1(r=0.999 1);平均回收率分别为101.6%(RSD=1.62%),99.7%(RSD=1.76%),97.4%(RSD=1.19%),99.9%(RSD=1.52%),102.2%(RSD=1.56%)。结论 该方法操作简便、快速,结果准确,可用于通脉颗粒的质量控制。 相似文献
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离子色谱法测定氯化琥珀胆碱原料及注射液中的氯化胆碱和氯化琥珀酰单胆碱 总被引:1,自引:1,他引:0
目的 采用离子色谱法测定氯化琥珀胆碱原料及注射液中的氯化胆碱和氯化琥珀酰单胆碱。方法 采用Dionex RFICTM Ionpac CS17色谱柱(4 mm×250 mm),以甲烷磺酸溶液为流动相进行梯度洗脱,流速为1.0 mL·min-1,采用抑制电导检测器进行测定。结果 氯化胆碱、氯化琥珀酰单胆碱浓度分别在18.0~562.8 μg·mL-1(r=0.999 9)和14.4~449.8 μg·mL-1(r=0.999 9)内线性关系良好,定量限均为0.01 μg·mL-1。原料中氯化胆碱、氯化琥珀酰单胆碱回收率分别为103.4%~105.7%和102.4%~107.1%;注射液中氯化胆碱、氯化琥珀酰单胆碱回收率分别为95.6%~100.2%和94.4%~103.5%。结论 该方法专属性强、准确、简便、快速,适用于氯化琥珀胆碱原料及制剂中的有关物质测定。 相似文献
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目的 建立测定复方氨基酸注射液中蛋氨酸亚砜含量的方法。方法 采用邻苯二甲醛(O-phthaladehyde,OPA)柱前衍生HPLC。色谱柱为Agilent ZORBAX Eclipse AAA C18柱(150 mm×4.6 mm,5µm),检测波长为338 nm,流动相A为0.04 mol·L-1磷酸二氢钠溶液(调节pH至7.8),流动相B为乙腈-甲醇-水(45:45:10),梯度洗脱,流速为2.0 ml·min-1,柱温为40℃,供试品溶液与OPA衍生剂及硼酸盐缓冲液按设定程序自动混匀后进样。结果 蛋氨酸亚砜的质量浓度线性范围为0.000 5~0.050 0 mg·mL-1(R=0.999 9);定量限为0.250 5 μg·mL-1,检测限为0.083 5 μg·mL-1;精密度、稳定性、重复性试验的RSD<3.0%;平均回收率为99.1%(RSD=1.33%,n=9)。结论 该方法操作简便,可用于复方氨基酸注射液中蛋氨酸亚砜的含量测定。 相似文献
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Manishkumar B. Patel Uma Harikrishnan Nikunj N. Valand Nishith R. Modi Shobhana K. Menon 《Archiv der Pharmazie》2013,346(3):210-220
A series of novel cationic fullerene derivatives bearing a substituted‐quinazolin‐4(3H)‐one moiety as a side arm were synthesized using the 1,3‐dipolar cycloaddition reaction of C60 with azomethine ylides generated from the corresponding Schiff bases of substituted quinazolinones. The synthesized compounds 5a – f were characterized by elemental analysis, FT‐IR, 1H NMR, 13C NMR, and ESI‐MS and screened for their antibacterial activity against Mycobacterium tuberculosis (H37RV) and antimicrobial activity against selected Gram‐positive (Staphylococcus aureus and S. pyogenes) and Gram‐negative (Pseudomonas aeruginosa, Klebsiella pneumonia and Escherichia coli) bacterial and fungal strains (Candida albicans, Aspergillus clavatus, and A. niger), respectively. All the compounds exhibited significant activity, with the most effective compounds having MIC values and zones of inhibition comparable to those of standard drugs. 相似文献
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Antonios E Goulas Panagiota Zygoura Andreas Karatapanis Dimitris Georgantelis Michael G Kontominas 《Food and chemical toxicology》2007,45(4):585-591
Food-grade polyvinyl chloride (PVC) cling-film containing 5.3% (w/w) di(2-ethylhexyl) adipate (DEHA) and 3.0% (w/w) acetyltributyl citrate (ATBC) plasticizers was used to wrap halawa tehineh (halva) samples. Samples were split into two groups and stored at 25+/-1 degrees C. One group was analyzed for DEHA and ATBC content at intervals between 0.5 and 240h of contact (kinetic study) and a second group was cut into slices (1.5mm thick) after 240h of halva/PVC contact and was analyzed for DEHA and ATBC content (penetration study). Determination of both plasticizers was performed using a direct gas chromatographic (GC) method after extraction of DEHA from halva samples. DEHA readily migrated into halva samples: the equilibrium amount of DEHA in halva (3.31mg/dm(2) film or 81.4mg/kg halva) corresponding to a loss of 54.7% (w/w) DEHA from PVC film. This value is slightly higher than the limit of 3mg/dm(2) of film surface set by the European Union for DEHA. The equilibrium amount of ATBC in halva was 1.46mg/dm(2) (36.1mg/kg) corresponding to a loss of 42.7% ATBC from PVC film. With regard to the penetration of both placticizers into halva samples, migration of DEHA was detectable up to the 7th slice beneath the surface of halva (total depth 10.5mm) while the migration of ATBC was detectable up to the 5th slice (total depth 7.5mm). 相似文献
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Selen Yegenoglu Dilek Aslan Sefik Evren Erdener Aylin Acar Nazmi Bilir 《Substance use & misuse》2013,48(3):405-414
This study, performed in two phases, compared the smoking status of first- and last-year pharmacy students and identified underlying factors of smoking using both “quantitative” and “qualitative” research techniques. The quantitative phase was a cross-sectional study with 207 students (of these, 102 were first-year and 105 were last-year students). The mean age at which first-year students tried tobacco/tobacco products was 14.1 ± 3.2 and for last-year students, 16.0 ± 2.4. The students completed an 18-item questionnaire at the end of the spring semester in May 2004. Chi-square and t-test analyses were used for statistical comparisons. Furthermore, focus group discussion techniques were used to find out the underlying factors of smoking in the second phase. 相似文献
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《Drug metabolism and pharmacokinetics》2018,33(2):118-124
ASP7991 is a calcimimetic that acts on the calcium-sensing receptor on parathyroid cell membranes and suppresses parathyroid hormone (PTH) secretion in the treatment of secondary hyperparathyroidism. The mass balance and metabolite profile of [14C]ASP7991 were investigated in six healthy male subjects after a single oral dose of [14C]ASP7991 [1 mg, 18.5 kBq (500 nCi)] in solution. [14C] radioactivity in plasma, urine and feces was analyzed using Accelerator mass spectrometry. ASP7991 was rapidly absorbed, metabolized and excreted. Mean recovery of [14C] radioactivity in urine and feces was 30.08% and 49.31%, respectively, and mean total recovery of [14C] radioactivity was 79.39%. The majority of [14C] radioactivity in urine and feces was excreted within the first 72 h following administration. Seven metabolites were detected in plasma, urine and feces samples, and their structures were determined by mass spectrometry. The main metabolic pathways of ASP7991 in humans were predicted to be N-dealkylation, followed by N-acetylation and taurine conjugation to a carboxylic acid moiety. Our findings show that a mass balance study using micro radioactivity doses is suitable for elucidating the pharmacokinetics of the absorption, metabolism and excretion of administered drugs. 相似文献
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嵌合抗原受体T细胞(CAR-T)疗法极大地改变了癌症的治疗前景,细胞因子释放综合征(CRS)是病理性免疫系统激活的严重全身炎症反应,也是CAR-T治疗过程中最常见且致命的毒性反应。目前CRS机制尚未完全阐明,临床前研究的实验模型主要包括异种移植免疫缺陷小鼠模型、同源小鼠模型、转基因小鼠模型、人源化小鼠模型和非人灵长类动物模型。由于种属差异且缺乏体外细胞模型,临床前预测CAR-T细胞引起CRS的风险仍是亟待解决的问题。从CRS的相关指导原则及法规、机制及临床前安全性评价方法和模型3个方面对CAR-T诱发的CRS进行综述,以期为CAR-T细胞治疗产品的临床前安全性评价策略提供新的思路。 相似文献
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目的 探讨了 NO/ NOS和 ET在冠心病患者中的变化。方法 分别应用生化法和放免法检测了3 9例冠心病患者血 NO/ NOS和 ET含量 ,并与 3 5名正常健康人作对照。结果 冠心病患者血 NO水平低于正常人 ( P<0 .0 5 ) ,NOS和 ET水平高于正常人 ( P<0 .0 1)。结论 NO/ NOS和 ET水平的变化与冠心病的发生与发展密切相关 相似文献
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