KMnO4-钙指示剂-罗丹明B化学发光法测定对乙酰氨基酚的含量

目的建立快速、准确测定对乙酰氨基酚的流动注射化学发光新方法。方法酸性条件下,KMnO_4可氧化钙指示剂产生化学发光,罗丹明B对此发光有较强的增敏,对乙酰氨基酚的存在抑制体系发光,基于此结合流动注射技术建立了一种新的测定对乙酰氨基酚含量的化学发光法。结果在优化的实验条件下,在5.0×10-7-1.0×10-5g/mL范围内,对乙酰氨基酚的质量浓度与化学发光信号的降低值有较好的线性关系,检出限(S/N=3)为7.0×10-8g/mL,对1.0×10-6g/mL对乙酰氨基酚进行11次平行测定,其相对标准偏差为2.2%。结论本方法简便、快速、准确,用于片剂中对乙酰氨基酚含量的测定,得到较满意的结果。     

流动注射化学发光法测定吩噻嗪类药物

目的确定以鲁米诺-高碘酸钾发光体系测定吩噻嗪类药物的化学发光分析方法。方法在碱性介质中,盐酸氯丙嗪和盐酸异丙嗪对鲁米诺-高碘酸钾发光体系有明显的增敏作用,且增敏效果与其浓度呈良好的线性关系。基于此,建立了盐酸氯丙嗪和盐酸异丙嗪的流动注射化学发光分析方法。结果在优化的实验条件下,盐酸氯丙嗪和盐酸异丙嗪的线性范围分别为3.0×10-9-1.0×10-6g/mL和3.0×10-8-7.0×10-5g/mL,检测限分别为5.0×10-10g/mL和7.3×10-9g/mL。结论本方法简便、快速、准确、灵敏度高、线形范围宽,应用于相应注射剂和片剂分析,并与药典方法进行对照,结果令人满意。     

多敏灵片中咖啡因和盐酸多塞平含量的测定

目的建立高效液相色谱法,测定多敏灵片中咖啡因、盐酸多塞平的含量。方法采用高效液相色谱法,以Kromasil C18(250 mm×4.6 mm,5μm)为分析柱,流动相为甲醇-水-三乙胺(75∶25∶1),流速1 mL/min,检测波长295 nm,柱温为室温。结果咖啡因、盐酸多塞平与其他组分分离良好,且不受其他成分的干扰;咖啡因回归方程为:Y=196 604X+218 976(r=0.999 8,n=5),咖啡因在0.08~0.24μg的范围内线性关系良好;盐酸多塞平回归方程为:Y=60 158X+58 230(r=0.999 9,n=5),盐酸多塞平在0.04~0.12μg的范围内线性关系良好。方法的平均回收率分别为99.06%、96.67%,精密度(RSD)值分别为1.04%、1.13%。结论本方法操作简便、快速、准确、灵敏,适用于多敏灵片的含量测定。     

奋乃静药物的流动注射化学发光测定方法的建立

目的建立快速测定奋乃静的流动注射化学发光新方法。方法在硝酸介质中,奋乃静能被硫酸铈氧化生成发光物质奋乃静砜,从而产生化学发光。基于此,建立了奋乃静的流动注射化学发光分析方法。结果在优化的实验条件下,不用任何发光增敏剂,奋乃静在1.0×10-7-7.0×10-5g/mL范围内与化学发光强度呈良好的线性关系,检出限(3σ)为8.0×10-8g/mL,对1.0×10-6g/mL的奋乃静进行了11次平行测定,其相对标准偏差为1.8%。结论本方法简便、快速、准确、灵敏度高、线形范围宽,应用于奋乃静片剂分析,并与药典方法进行对照,结果满意。     

流动注射-化学发光法测定氢化可的松

目的确定以高锰酸钾-亚硫酸钠体系测定氢化可的松的流动注射-化学发光分析方法。方法在酸性条件下,氢化可的松对高锰酸钾-亚硫酸钠体系发光反应具有明显的增敏作用。据此,建立了流动注射化学发光测定氢化可的松的分析方法。结果在优化的实验条件下,氢化可的松质量浓度在1.0×10-9-1.0×10-6g/mL范围内与发光强度呈良好的线性关系,检出限(3R)为4.0×10-10g/mL,对氢化可的松进行11次平行测定,其相对标准偏差为2.2%。结论本方法应用于注射液中氢化可的松含量的测定,快速、准确、简便,灵敏度高、线性范围宽。     

流动注射-化学发光法测定阿昔洛韦和更昔洛韦

目的确定以Ce(IV)-罗丹明B体系测定制剂中阿昔洛韦和更昔洛韦的流动注射-化学发光(FI-CL)分析方法。方法硫酸介质中Ce(IV)与阿昔洛韦/更昔洛韦发生氧化-还原反应而产生化学发光,罗丹明B可显著增强其发光信号,且增敏效果与阿昔洛韦/更昔洛韦浓度呈一定的线性关系。据此,建立了测定注射剂中阿昔洛韦和更昔洛韦的流动注射-化学发光新方法。结果阿昔洛韦在3.0×10-5g/L-7.0×10-2g/L范围内呈线性关系,检出限为1.56×10-5g/L;更昔洛韦在5.0×10-5g/L-7.0×10-2g/L范围内呈线性关系,检出限为2.35×10-5g/L。通过对质量浓度为1.0×10-3g/L的阿昔洛韦和更昔洛韦分别进行的11次平行测定,其相对标准偏差(RSD)分别为2.08%和2.83%。结论该方法线性范围宽、灵敏度高,简便快速,也是目前首次采用流动注射-化学发光法对更昔洛韦含量的测定。     

6005A铝合金焊接接头的腐蚀行为

采用浸泡试验和电化学方法研究了6005A铝合金焊接接头在不同介质环境中的腐蚀行为,采用光学显微镜、扫描电子显微镜、电子能谱分析了焊缝微观组织和成分的变化.结果表明,由于ER5356焊丝Mg含量较高,致使焊缝中Mg含量高于母材,因此焊缝耐蚀性能低于母材;在浸泡试验中焊缝发生均匀腐蚀,表面呈多孔形貌,其对光线的反射明显弱于仅发生点蚀的母材,表现出焊缝发黑的现象;焊接接头在0.1 M NaCl、0.1 M Na2SO4和0.1 M NaNO3溶液中的腐蚀速度为VNaCl>VNa2SO4> VNaNO3.     

6005A铝合金焊接接头的腐蚀行为

采用浸泡试验和电化学方法研究了6005A铝合金焊接接头在不同介质环境中的腐蚀行为,采用光学显微镜、扫描电子显微镜、电子能谱分析了焊缝微观组织和成分的变化．结果表明,由于ER5356焊丝Mg含量较高,致使焊缝中Mg含量高于母材,因此焊缝耐蚀性能低于母材;在浸泡试验中焊缝发生均匀腐蚀,表面呈多孔形貌,其对光线的反射明显弱于仅发生点蚀的母材,表现出焊缝发黑的现象;焊接接头在0．1MNaCl、0．1MNa2SO4和0．1MNaNO3溶液中的腐蚀速度为VNaCl〉VNa2SO4〉VNaNO3.     

基于XRD分析的钢渣填料沥青混合料水稳定性研究

为探究钢渣矿物成分对沥青混合料性能的影响,本研究采用不同种钢渣,分别按0%、30%、60%和100%的掺量及陈化前后30%的两种K钢渣进行沥青混合料的水稳定性测试,并采用XRD进行成分分析。研究结果表明:相比于普通石灰岩矿粉及水泥,不同钢渣的硅酸盐矿物及CaO等活性成分含量差异较大,且其对沥青混合料性能的提升存在较大差异。马歇尔稳定度及劈裂强度提升28.0%～40.0%;K钢渣随掺量增加,活性成分含量提高,对混合料性能提升也略有提高,马歇尔稳定度及劈裂强度提升38.0%～40.0%;钢渣陈化后活性矿物成分减少,对沥青混合料的提升效果减弱;水稳定性随活性成分增多有所降低;K钢渣在30%掺量时,水稳定性及劈裂强度性能提升最显著。     

流动注射化学发光法测定何首乌中二苯乙烯苷的含量

目的　建立二苯乙烯苷的流动注射发光分析法。方法　二苯乙烯苷对鲁米诺 过氧化氢发光体系在pH =12的溶液中具有一定的抑制作用 ,且此抑制作用在一定范围内与二苯乙烯苷浓度间呈线性关系 ,借此建立了二苯乙烯苷的流动注射发光分析法。结果　此方法检出限为 6 .0× 10 -5g·L-1,线性范围为 1.0× 10 -4～ 1.6× 10 -2 g·L-1。对 1.1× 10 -4g·L-1二苯乙烯苷平行测定 11次 ,其相对标准偏差为 1.4 6 %。结论　本法简便、快速、准确 ,可作为何首乌中二苯乙烯苷含量的测定方法     

Capillary electrophoresis coupled with electrochemiluminescence for determination of cloperastine hydrochloride

Objective To investigate the electrochemiluminescence (ECL) behavior of cloperustine hydrochloride.Methods ECL intensity of tris (2,2'-bipyridyl) rutheniumo(Ⅱ) was enhanced, the method for the determination of dupernstine hydrochloride was established using capillary electrophoresis (CE) coupled with electrochemilumolinescence (ECL) detection. Results Under the optimum conditions, ECL intensity varied linearly with cloperastine hydrochloride concentration from 7.0×10-6 g/mL to 1.0×10-4 g/mL. The detection limit (S/N=3) was 8.05×10-7g/mL. he relative standard deviation of the ECL intensity and the migration time for 11 consecutive injections of 1.0 ×10-5g/mL cloperastine hydrochloride was 2.9% and 1.5%, respectively. This method was successfully applied to eloperastine hydrochloride tablet determination. Conclusion The method has been established, validated and applied for determination of cloperastine hydrochloride.     

Electrogenerated chemiluminescence sensor for the determination of metoclopramide using ordered mesoporous carbon for immobilizing tris(2, 2'-bipyridyl) ruthenium

A novel electrogenerated chemiluminescence (ECL) sensor for the determination of metoclopramide was developed by employing ruthenium complex as an ECL signal producer and an ordered mesoporous carbon (OMC) material as modified material. The ECL sensor was fabricated by adsorption ruthenium complex into a mixture of OMC and Nafion, which showed good electrochemical and ECL behaviors. It was found that the ECL intensity of the sensor fabricated was greatly enhanced in the presence of metoclopramide. Based on this finding, a highly sensitive and reproducible ECL method was developed for the determination of metoclopramide. The result showed that the ECL intensity was linear with the concentration of metoclopramide in the range from 1.0×10-10 to 5.0×10-7M and the detection limit was 3×10-11M. The ECL sensor exhibited a long-term stability and a fine reproducibility with relative standard deviation of 1.0 % for 1.0×10-10M metoclopramide in 18 continuous determinations. The developed method has been applied to the determination of metoclopramide in tablet samples with satisfactory results.     

DETERMINATION OF TETRACYCLINE AND OXYTETRACYCLINE BY FLOW-INJECTION CHEMILUMINESCENCE METHOD

Tetracycline and oxytetracycline are broad-spec-trumantibiotics.They are not only used in humanpathologies,but alsoin veterinary medicine,ani malnutrition and feed additives for cattle breeding.In the past few years,the deter mination meth-ods of tetracycline and oxytetracycline were repor-ted,which involved in difference spectrophotome-try[1],HPLC[2,3],spectrophotometry[4-7],HPLC-MS[8-9],spectrofluori metry[10],solid-phase extrac-tion[11]and kinetic methods.Recently,flow-injection CL met…     

Response surface optimization of microwave-assisted extraction for HPLC-fluorescence determination of puerarin and daidz

Microwave-assisted extraction was optimized with response surface methodology for HPLC-fluorescence determination of puerarin and daidzein in Radix Puerariae thomsonii.The optimized extraction procedure was achieved by soaking the sample with 70% methanol     

Capillary electrophoresis with inhibited electrochemiluminescent detection for the trace analysis of epinephrine and dopamine

In this paper, a novel electrochemiluminescent (ECL) detection approach was developed for highly sensitive detection of ECL inhibitors based on the ECL inhibition of Ru(bpy)32+/2-(Dibutylamino)ethanol (DBAE) system. A microfluidic ECL detection cell was fabricated to couple with the capillary electrophoresis system, the electrochemical system and the postcolumn injection system. Both Ru(bpy)32+ and DBAE solutions were injected directly to the working electrode surface by a micro-infusion system to obtain a high and stable ECL signal. The performance of this setup was demonstrated by the analysis of two typical ECL inhibitors, dopamine and epinephrine. Under the optimal conditions, the limit of detection (LOD) for dopamine and epinephrine was 50nM and 5nM respectively. The proposed method was also successfully used for the trace analysis of dopamine and epinephrine in human serum samples.     

Luminol-potassium permanganate chemiluminescence system for the determination of three anthracycline antibiotics

Objective To establish a flow-injection chemiluminescence method for the determination of doxorubicin, epirubicin and mitoxantrone and study its reaction mechanism. Methods In alkaline medium, chemiluminescence of luminol-potassium permanganate system could be inhibited obviously by anthracycline antibiotics. Combined with flow-injection technique, a new chemiluminescence method for determining the anthracycline antibiotics was set up. The chemiluminescence mechanism of the luminol-potassium permanganate system was also discussed. Results Under optimal conditions, the good linear ranges of doxorubicin, epirubicin and mitoxantrone were 5.0×10-9-1.0×10-6g/mL, 1.0×10-9-1.0×10-5g/mL and 3×10-9-1.0×10-6g/mL, respectively. The detection limits of doxorubicin, epirubicin and mitoxantrone were 3.0×10-9g/mL, 5.0×10-8g/mL and 2.0×10-9g/mL, respectively. During eleven repeated inter-day and intra-day precision tests of 1.0×10-6g/mL samples, the relative standard deviations corresponded to reference values of 3.0%, 2.8% and 2.1%. Conclusion The developed method is sensitive, accurate, rapid and of low cost. It can be applied to determine doxorubicin hydrochloride, epirubicin hydrochloride and mitoxantrone hydrochloride in injection preparations.     

钙拮抗剂尼群地平的反相高效液相色谱分析及其在家兔体内的分布

对兔血浆及组织器官中钙拮抗剂尼群地平的分析方法进行了研究，建立了反相高效液相色谱（RP-HPLC）的内标测定法。样品在弱碱性条件下经环已烷-异丙醇（96．5：3．5）提取，用YWGC18反相柱，以地尔硫作内标，甲醇：50mmol／L磷酸盐缓冲液（70：30）pH6．8为流动相，UV236nm检测。方法最低检测限约为10ng，血药浓度在21．6～216μg／L之间，尼群地平的量与其峰面积比值之间，线性关系良好，回归方程为Y＝0．00672X－0．013，r＝0．9958。方法回收率95．4％～98．1％，RSD＜4．63％。　用该分析方法测定了家兔口服尼群地平2h后在主要脏器体液中的分布。