HPLC测定氨咖黄敏胶囊中对乙酰氨基酚和咖啡因的含量

目的　建立同时测定氨咖黄敏胶囊中对乙酰氨基酚和咖啡因含量的高效液相色谱法。方法　采用ODS柱 ,流动相 :甲醇 -水 (40∶6 0 ) ,流速 1.0ml/min ,检测波长 2 17nm ,外标法计算。结果　线性范围分别为对乙酰氨基酚 12 0～ 80 0 μg·ml-1,r=0 .9998;咖啡因 12～ 80 μg·ml-1,r =0 .9999,回收率分别为对乙酰氨基酚 10 0 .5 % ,RSD为 0 .2 % ,咖啡因 99.8% ,RSD为 0 .5 %。结论　本法分离效果好 ,辅料无干扰 ,快速、简便。     

Caffeine has a small effect on 5-km running performance of well-trained and recreational runners

The purpose of this study was to investigate if caffeine ingestion improves 5-km time-trial performance in well-trained and recreational runners. Using a double-blind placebo-controlled design, 15 well-trained and 15 recreational runners completed two randomized 5-km time-trials, after ingestion of either 5mgkg(-1) of caffeine or a placebo. Caffeine ingestion significantly improved 5-km running performance in both the well-trained and recreational runners. In comparison to the placebo trial, the caffeine trial resulted in 1.1% (90% CI 0.4-1.6) and 1.0% (0.2-2%) faster times for the well-trained and recreational runners. Reliability testing of the recreational runners indicated a test-retest error of measurement of 1.4%. We conclude that caffeine ingestion is likely to produce small but significant gains in 5-km running performance for both well-trained and recreational runners.     

以双氯酚酸为探针采用高效液相色谱法快速测定CYP4502C9的酶活性

目的建立一种快速、高效的以双氯酚酸作为探针药物评价细胞色素P4502C9（CYP2C9）酶活性的高效液相色谱．紫外检测方法。方法色谱柱为Agilent Zorbax SB—C18柱（50mm×4．6mmI．D．,5μm）;流动相为乙腈（含0．01％七氟丁酸）-水（含0．01％七氟丁酸）（65：35,V／V）,流速2．0mL/min;检测波长为280nm。双氯酚酸与人CYP2C9酶在37℃温孵适当时间后,加入100μL乙腈-冰乙酸（94：6,V／V）终止反应,10000g离心后取上清液进样分析测定。结果4’-羟基双氯酚酸的保留时间为1．35min,线性范围为1．00—200μmol·L^-1（r=0．9999）,最低定量限为1．00μmol·L^-1,回收率为99．5％-100．8％;双氯酚酸的保留时间为2．25min,线性范围为1．00～200μmol·L^1（r=0．9999）,最低定量限为1．00μmol·L^-1,回收率为99．3％～101．1％。两者的日内、日间RSD均〈15％,温孵体系中的其他内源性物质不干扰测定。结论该方法快速、稳定、灵敏度高,适合体外双氯酚酸及其代谢物4’-羟基双氯酚酸的测定,可应用于体外CYP2C9酶活性的评价及酶动力学的研究。     

效应面法优化浊点萃取-HPLC测定小鼠脑组织中蛇床子素含量

目的建立基于浊点萃取同时测定小鼠脑组织中蛇床子素含量的HPLC法。方法以非离子表面活性剂Triton X-114为浊点萃取剂,考察了Triton X-114浓度、NaCl浓度、萃取温度和时间等对蛇床子素萃取有影响的因素,并进一步采用效应面法分析优化实验条件。同时建立了HPLC法测定小鼠脑组织中蛇床子素含量的分析方法。结果蛇床子素在最佳萃取条件下的萃取率为93.8%。RSD≤5.6%,加样回收率为97.2%。结论采用浊点萃取法代替传统有机溶剂萃取小鼠脑组织中蛇床子素,操作简便,萃取率高,方法重复性好,可用于蛇床子素体内药代动力学的研究。     

RP-HPLC法测定妇炎平泡腾片中盐酸小檗碱的含量

目的用高效液相色谱法测定妇炎平泡腾片中盐酸小檗碱的含量。方法用十八烷基硅烷键合硅胶为填充剂;乙腈-0.033mol·L^-1磷酸二氢钾溶液（35∶65）为流动相;检测波长为424nm;流速：1.0ml/min。结果盐酸小檗碱进样量在0.0388～0.776μg范围内呈良好线性关系,平均加样回收率为100.23%（RSD=1.5%）。结论该法快速简便,结果准确可靠。     

高效液相色谱法测定大鼠血清中艾司洛尔的含量

目的：建立高效液相色谱法（HPLC）测定因清中艾司洛尔浓度的方法。方法：以甲醇－冰醋酸－0．2％醋酸钠（60：1：40）为流动相，流速1．0ml/min，检测波长为280nm。结果：在10－600ug/ml^-1范围内样品色谱峰高与血清药物浓度呈良好的线性关系，r=0.9998，日内及日内RSD分别测得为3．05％,4．43％，平均加样回收率为100．45％，血清中药物最低检测浓度为13．3ug.L^-1。结论：本方法适于艾司洛尔的血药浓度监测。     

Instrumental set-up as a factor influencing the variability of retention index values in high pressure liquid chromatography

Summary The influence of different laboratory set-ups on HPLC retention index values of selected acidic and basic drugs was investigated. The RI values of drugs were calculated using the alkyrarylketone scale. Two columns filled with different batches of the same Hypersil ODS phase were consecutively used in two laboratories under identical conditions, but using different instrumentation. The study showed that the different laboratory set-ups influence the precision of RI values, and the differences in column filling affect the accuracy.     

Saline-Enhanced Hepatic Radiofrequency Ablation Using a Perfused-Cooled Electrode: Comparison of Dual Probe Bipolar Mode with Monopolar and Single Probe Bipolar Modes

Objective

To determine whether saline-enhanced dual probe bipolar radiofrequency ablation (RFA) using perfused-cooled electrodes shows better in-vitro efficiency than monopolar or single probe bipolar RFA in creating larger coagulation necrosis.

Materials and Methods

RF was applied to excised bovine livers in both bipolar and monopolar modes using a 200W generator (CC-3; Radionics) and the perfused-cooled electrodes for 10 mins. After placing single or double perfused-cooled electrodes in the explanted liver, 30 ablation zones were created at three different regimens: group A; saline-enhanced monopolar RFA, group B; saline-enhanced single probe bipolar RFA, and group C; saline-enhanced dual probe bipolar RFA. During RFA, we measured the tissue temperature at 15mm from the electrode. The dimensions of the ablation zones and changes in the impedance currents and liver temperature during RFA were then compared between the groups.

Results

The mean current values were higher for monopolar mode (group A) than for the bipolar modes (groups B and C): 1550±25 mA in group A, 764±189 mA in group B and 819±98 mA in group C (p < 0.05). The volume of RF-induced coagulation necrosis was greater in group C than in the other groups: 27.6±2.9 cm³ in group A, 23.7±3.8 cm³ in group B, and 34.2±5.1 cm³ in group C (p < 0.05). However, there was no significant difference between the short-axis diameter of the coagulation necrosis in the three groups: 3.1±0.8 cm, 2.9±1.2 cm and 4.0±1.3 cm in groups A, B and C, respectively (p > 0.05). The temperature at 15 mm from the electrode was higher in group C than in the other groups: 70±18℃ in group A, 59±23℃ in group B and 96±16℃ in group C (p < 0.05).

Conclusion

Saline-enhanced bipolar RFA using dual perfused-cooled electrodes increases the dimension of the ablation zone more efficiently than monopolar RFA or single probe bipolar RFA.     

HPLC-电化学法测定胞磷胆碱钠注射液中游离胆碱含量

目的建立胞磷胆碱钠注射液中游离胆碱含量测定方法。方法采用高效液相色谱电化学检测法,专用色谱柱（ESA ACH-3,250 mm×3 mm ID）和固相胆碱氧化酶反应器（ESA ACH-SPR,3 cm）,M5040分析电极和5300型电化学检测器,柱温：35℃,流速：0.35 ml.min-1。结果游离胆碱在0.12～2.89μg.ml-1范围内呈良好线性关系,r=0.9999,平均回收率为100.0%,RSD为2.7%（n=6）。结论该方法简便可行,重复性好,可用于胞磷胆碱钠注射剂中游离胆碱含量测定。     

Percutaneous Microwave Ablation of Renal Tumors Using a Gas-Cooled 2.4-GHz Probe: Technique and Initial Results

The feasibility, safety, and preliminary effectiveness of microwave ablation (MWA) in the treatment of renal tumors using a high-powered, carbon dioxide–cooled probe were evaluated. There were 15 tumors treated in 14 patients. Computed tomography was performed immediately after MWA, and follow-up imaging was performed to evaluate for recurrence. Immediate technical effectiveness was 100%. One complication involved the formation of a renal artery pseudoaneurysm. At follow-up (mean interval, 12.5 wk) evaluation, 14 of 15 (93.3%) tumors demonstrated complete necrosis. MWA is a safe, effective treatment modality; larger studies are warranted to demonstrate long-term oncologic outcomes.