HPLC法同时测定血浆地西泮及其代谢物浓度

目的 :建立同时测定血浆中地西泮及其代谢物浓度的方法。方法 :选用ZORBAXRP C18柱 (15 0mm× 4 6mm ,5 μm) ;甲醇 - 2 5mmol·L-1醋酸铵溶液 (6 0∶4 0 ,V/V)作流动相 ;流速 0 8mL·min-1;检测波长 2 30nm。取血浆样品 0 5mL ,在碱性条件下用二氯甲烷 -正己烷提取 ,HPLC检测。结果 :本法对替马西泮、去甲地西泮和地西泮 3种物质的最低检测限均为 2 μg·L-1,线性范围为 10～ 15 0 0 μg·L-1;奥沙西泮的最低检测限为 5 μg·L-1,线性范围为 2 0～ 15 0 0 μg·L-1。回收率均接近 10 0 % ,日内、日间RSD <5 %。结论 :本法能同时测定血浆中地西泮及其代谢物浓度 ,具有重现性好 ,灵敏、可靠 ,可用于地西泮中毒的监测     

反相高效液相色谱-质谱法测定人血浆中阿坎酸钙浓度

目的反相高效液相色谱-质谱法测定人血浆中阿坎酸钙浓度.方法采用API 3 000 LC-MS/MS液质联用系统.Phenomenex Gemini C18分析柱(50 mm×3.0 mm,3 μm),流动相为10 mmol·L-1乙酸铵-甲醇(95∶5,氨水调pH至7.4),流速为0.2 mL·min-1.样品用乙腈沉淀蛋白,离心,定量取上清液挥干,二氯甲烷洗后进样,按外标法定量.结果标准曲线在2～2 048 μg·L-1范围内有良好线性,最低定量限为2.0 μg·L-1,阿坎酸钙的保留时间为2.4 min,日内RSD＜4.0%,日间RSD＜11.6%,方法回收率为80%～104%,预处理回收率为83.6%～94.4%.结论本法具有快速简便、灵敏准确等特点,适用于阿坎酸钙血药浓度测定及药动学、生物利用度研究.     

高效液相色谱法同时测定血浆和尿中阿普唑仑和硝西泮浓度

目的 建立高效液相色谱法测定血浆及尿中阿普唑仑、硝西泮浓度. 方法 采用Agilent Eclipse XDB C₁₈色谱柱（4.6 mm×150 mm, 5 μm ）,以甲醇 水（60：40）为流动相,流速1.0 mL&#8226;min^-1,检测波长：254 nm. 结果 硝西泮、阿普唑仑和内标物（地西泮）的出峰时间分别为4.0,5.1和8.6 min,分离效果较好; 硝西泮、阿普唑仑质控3种浓度（4.0,8.0,16.0 μg&#8226;mL^-1）日内和日间的RSD,血浆样品均＜6.89%,尿样均＜5.80%,血浆阿普唑仑和硝西泮回收率分别为94.33%～96.09%和95.12%～97.89%,尿液阿普唑仑和硝西泮回收率分别为87.59%～91.24%和88.92%～93.65%,血浆及尿样样品线性范围为2.0～32.0 μg&#8226;mL^-1. 结论 该条件可对血浆和尿中阿普唑仑、硝西泮快速定量检测.     

HPLC法测定血浆及尿中硝基安定浓度

目的建立高效液相法测定血及尿中硝基安定的浓度。方法采用Agilent Eclipse XDB-C18色谱柱以甲醇-水（70∶30）为流动相,流速1.0mL·min-1,检测波长254nm。结果该法分离效果较好;硝基安定质控3种浓度（4.0,8.0,16.0μg·mL^-1）日内和日间的RSD,血浆样品均小于7%,尿样均小于5%,血浆回收率为87.13%～92.15%,尿回收率为89.82%～92.75%,血浆及尿样样品线性范围为4.0～64.0μg·mL^-1,相关系数在0.9972。血浆、尿样中硝基安定最低检出限为4.0μg·mL^-1。结论此方法可对硝基安定进行中毒药物快速检测并定量。     

RP-HPLC法测定血浆罗格列酮浓度

目的 :建立RP HPLC法测定血浆罗格列酮浓度。方法 :采用shim packCLC ODS柱及荧光检测 ,激发波长为 2 5 0nm ,发射波长为 370nm。以 10mmol·L-1乙酸铵 甲醇 ( 12∶40 ) ,用浓氨水调 pH至 8.0 0为流动相 ,流速为 0 .7mL·min-1。样品用二氯甲烷提取 ,按内标法定量。结果 :标准曲线在 10 .2 2～ 2 0 4.4μg·L-1范围内有良好线性关系 (r =0 .99994) ,最低定量浓度为 10 .2 2 μg·L-1,平均方法回收率为 97.6 7% ,日内RSD小于 4.0 % ,日间RSD小于 8.0 %。结论 :本法具有快速简便、灵敏准确等特点 ,适宜血浆中罗格列酮的浓度测定。     

高效液相色谱法测定人血清中地西泮血药浓度及临床监测

目的 建立人血清中地西泮浓度测定的高效液相色谱法(HPLC),并用该法测定临床病人静脉滴注地西泮后的血药浓度.方法 人血清样品采用正戊烷萃取进行分析.色谱柱:SB-C18色谱柱(150 mm×4.6 mm,5 μm),流动相为甲醇-水-四甲基乙二胺-冰醋酸(670:330:2.2:1.76),柱温:40 ℃,流速:0.8 mL·min-1,检测波长:254 nm,进样量:20 μL.以氯氮平作为内标物.结果 地西泮在10~1 200 μg·L-1浓度范围内,峰面积与其浓度呈良好的线性关系(r=0.998 47),定量下限为10 μg·L-1.地西泮的高、中、低3种浓度相对平均回收率>95%,提取回收率均>70%,日内、日间的RSD均<15%(n=5).地西泮稳定性考察RSD均<15%(n=5).地西泮线性方程:Y=2 205.2X+1 876.1(r=0.998 47).临床20例病人分别滴注地西泮20 mg,1 d 2次,前5 d早晨治疗前采血均检测出地西泮血药浓度.结论 该方法灵敏度高,操作简便、快速、准确,可用于人血清中地西泮血药浓度监测,并为临床病人个体化给药提供参考.     

液相色谱法测定人血浆和尿中的头孢布腾

头抱布腾（ceft止＂ten）是新的口服头抱菌素。本文介绍了可同时测定头抱布腾及其代谢物（反式异构体）的液相色谱（LC）法，用两种LC法分别评价了其药动学和人血浆与尿排泄物。稀血浆样品在蛋白沉淀前直接注入到反相柱上，稀尿样用转换柱，样品通过自动联机纯化处理。在临床有关浓度范围内两种方法测定结果相似，血浆浓度为0．1～50ug·mL－’，尿样浓度为0．5～60urn·mL’。血浆和尿中头抱布腾的检测限的相对标准差（RSD）（20％，其最低检测浓度分别为01和OSug·mL－‘。血浆日内和日间分析的RSD＜12％，尿样为7％。本法已成功地…     

RP-HPLC测定大鼠血浆中水飞蓟宾的浓度

目的　测定大鼠血浆中水飞蓟宾的浓度。方法　用RP -HPLC。样品以叔丁基甲醚提取 ,色谱柱为PoresphereC18柱 (4.0mm× 2 5 0mm ,5 μm) ,流动相为甲醇 水 0 .0 5mol·L-1磷酸二氢钾 (2 0∶10∶7) ,流速为 1.0ml·min-1,检测波长为 2 88nm ,温度为室温。结果　大鼠血浆中成分对水飞蓟宾的测定无干扰 ;在 0 .0 0 6 1～ 3.12 5 μg·ml-1浓度范围内呈现良好的线性关系 ,r=0 .9992 ;血浆中水飞蓟宾的最低检测浓度为 6ng·ml-1,平均回收率为10 7.0 0 % ,日内RSD≤ 8.19% ,日间RSD≤ 13.78%。结论　该法样品处理简便 ,灵敏度高 ,结果准确。     

HPLC法同时测定健康人血浆中贝那普利及其代谢物贝那普利拉的浓度

目的建立一种灵敏度较高的高效液相色谱法,可同时测定健康人血浆中贝那普利及其代谢物贝那普利拉的浓度。方法流动相用0.02mol·L-1磷酸二氢钾缓冲液-乙腈(7∶3)(pH2.6),用取梯度洗脱法,血浆样本用C8固相小柱萃取,紫外检测波长为237nm。结果贝那普利:在0.06～2μg·mL-1,线性关系良好;最低检测限为0.03μg·mL-1;日内RSD≤6.3%,日间RSD≤4.0%;提取回收率在73%～78.5%(n=5),相对回收率在93.2%～101.3%。贝那普利拉:在0.06～2μg·mL-1,线性关系良好;最低检测限为0.03μg·mL-1;日内RSD≤8.5%,日间RSD≤6.0%;提取回收率在67.7%～74.1%(n=5),相对回收率在95.6%～103.2%。结论本方法灵敏度高、重现性好,可用于贝那普利人体生物利用度和药代动力学研究。     

HPLC和微生物法测定万古霉素的血药浓度

目的比较HPLC和微生物法测定万古霉素血药浓度的差异。方法30名病人静脉滴注万古霉素1.0 g,1次·d-1,分别用HPLC和微生物法测定用药前后的血药浓度。结果HPLC法在5.0～80 μg·mL-1浓度内线性关系良好,回收率97.3%～101.6%,日内、日间RSD分别为1.74%～4.06%和1.22%～4.21%;微生物法线性范围在5.0～60 μg·mL-1,回收率：98.2%～100.8%,日内、日间RSD分别为4.22%～5.51%和4.59%～6.49%。结论2种测定方法回收率和精密度均符合要求,测得的血药浓度无显著性差异。     

不同厂家安定片的体外溶出度比较

不同厂家安定片的体外溶出度比较裴云萍，葛卫红，李建平（南京市鼓楼医院药剂科，南京２１０００８）摘要采用转篮法研究了四个厂家６个批号安定片的体外溶出度，实验数据用威布尔分布模型拟合，求得Ｔ＿ｄ、Ｔ＿（５０）、ｍ．结果表明：不同厂家生产的安定片溶出度差异...     

Diazepam protects against the enhanced toxicity of cocaine adulterated with atropine

We examined the toxicity of cocatropine (cocaine/atropine mixture) and the therapeutic potential of diazepam on some behavioral and physiological parameters in rats. Atropine (20 and 60 mg/kg) or cocaine (40 mg/kg) alone did not induce any seizure or death, but the combination significantly increased both, after both acute and binge treatment. There was a significant increase of EEG mean total spectral power in cocatropine- in comparison with cocaine-treated animals. Hyperlocomotion was observed in non-seizuring rats treated with cocaine or cocatropine. Cocaine, atropine 60, and cocatropine (40 + 20 and 40 + 60) all induced hyperthermic effects in non-seizuring rats, while cocatropine (40 + 60)-seizuring animals had hypothermia. An initial hypertensive and tachycardiac effect within 15 min was followed by a secondary fall in the cocatropine (40 + 60) group. Cocatropine toxicity was partially or fully reversed by diazepam (5 mg/kg), given intraperitoneally after the first seizure. The present findings provide, for the first time, details of a synergistic toxic effect of the cocaine/atropine mixture and of the potential of diazepam for treating cocatropine-related hospital emergencies.     

地西泮与缩宫素联合应用在产程缩短中的效果观察

目的探讨地西泮与缩宫素联合应用在产程缩短中的治疗效果。方法选取2009年2月至2010年11月来四川省内江市威远县人民医院进行分娩的300例产妇做为研究对象,并将其随机分为对照组(缩宫素治疗组)150例和观察组(地西泮与缩宫素联合应用组)150例,后将两组产妇的产程、角色适应情况进行统计及比较。结果观察组的产程时间短、产妇的角色适应高于对照组;而产后1周及2周后母婴的基本情况与对照组相比较,P<0.05或P<0.01,有显著性差异或有非常显著性差异。结论地西泮与缩宫素联合应用在产程缩短中的治疗效果明显高于单独使用缩宫素效果,是促进产程进展和无痛分娩的理想药物,应在临床推广及应用。     

高效液相色谱法测定地西泮的含量

目的建立测定地西泮含量的高效液相色谱法。方法以C18化学键和硅胶为固定相,甲醇-水(70∶30)为流动相,检测波长254 nm。结果地西泮进样量在0.523 5～3.141 0μg范围内与峰面积值线性关系良好,r=1.000(n=5);平均回收率为98.30%,RSD为0.54%(n=6)。结论高效液相色谱法简便、准确,可用于地西泮含量的测定。     

地西泮注射液含量的测定方法探讨

目的建立高效液相分析的外标法测定地西泮注射液含量的方法。方法采用C18色谱柱(KromasilC18(5μm)250mm×4.6mm),以甲醇-水(7∶3)为流动相,流速为1mL·min-1,检测波长为254nm。结果地西泮进样浓度在0.05～0.5g·L-1的范围内与峰面积呈良好的线性关系,相关系数为0.9999,平均回收率为100.1%。地西泮的定量限为2.4×10-5g·L-1,地西泮的检出限为4.8×10-6g·L-1。结论本方法操作简便快速,结果准确可靠。     

Diazepam in tardive dyskinesia

Tardive dyskinesia, a syndrome of involuntary motor movements, can be a permanent consequence of the long-term use of antipsychotic drugs. While there is no well-established drug treatment, case reports and the results of a few clinical studies suggest that drugs that facilitate the GABA-ergic system may decrease the abnormal movements. One such class of drugs is the benzodiazepines. We administered diazepam to 13 subjects in a 24-week, crossover design study. Tardive dyskinesia and psychopathology were assessed by blind raters using the Abnormal Involuntary Movement Scale and the Brief Psychiatric Rating Scale (BPRS). The means of all movement measurements improved from the baseline, with orofacial, subtotal, symptom severity, and total reaching significance. However, we were unable to demonstrate a drug effect; the patients improved to a similar degree whether or not they received diazepam. Their psychiatric disorders did not worsen with diazepam administration and, in fact, improved slightly; the activation factor of the BPRS was significantly improved over baseline. Our results suggest that diazepam is not effective in managing the movements of tardive dyskinesia and that behavior modification strategies be investigated to help patients control symptoms.     

Diazepam and presynaptic inhibition

This investigation clarifies the influence of diazepam upon the spinal cord. Certain spinal reflex alterations previously attributed to diazepam are influences of the vehicle used. Enhancement of presynaptic inhibition is the only spinal reflex activity found to result from the administration of diazepam. Inhibitory influences of diazepam are found to be directly related to the primary afferent depolarization, with no indication of postsynaptic influence. Picrotoxin and diazepam seem to act as antagonists at the same loci responsible for primary afferent depolarization. The spinal influence of diazepam is not mediated or altered by higher CNS structures. The doses required for spinal influence are comparable to those used in studies on the higher CNS.     

Onset and offset of the Diazepam stimulus complex

Rats were trained to discriminate 3.0 mg/kg diazepam from saline in a two lever operant procedure. The time from injection to test session was 30 minutes. The diazepam discrimination consisted of initial responses on the lever paired with saline, but after training shifted to the lever paired with diazepam (onset). When tested with saline immediately after injection, animals responded consistently on the saline lever throughout the test. A shift from the drug lever to the saline lever at a later time point was also observed (offset). In addition, it was not possible to establish a peripheral diazepam drug stimulus complex. The result show that diazepam exerts discriminative control from 10 to 210 minutes after intraperitonal injections, confirming a central action of the diazepam drug stimulus complex. The method might be useful in experimentation on drug control of lever selection.