测定奥美拉唑的流动注射化学发光新方法

目的 建立测定奥美拉唑的流动注射化学发光新方法.方法 当将奥美拉唑注入到高锰酸钾与鲁米诺反应的合并流中时,可检测到强的化学发光信号,结合流动注射技术对实验条件进行优化.结果在优化的实验条件下,即混合管长度:150cm,反应介质的碱度:0.15mol/L NaOH,鲁米诺的浓度:7.0×10-5mol/L,高锰酸钾的浓度:2.0×10-5mol/L以及试剂流速:2.8mL/min,奥美拉唑浓度在2.0×10-8～1.0×10-5g/mL范围内与相对化学发光强度具有线性关系;对浓度为1.0×10-7g/mL和1.0×10-6g/mL奥美拉唑溶液进行11次平行测定的相对标准偏差分别为1.0%和2.6%;该方法的检出限为3×10-9g/mL.结论该方法简单、快速、灵敏,适用于药物制剂中奥美拉唑的含量测定.     

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。     

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。     

流动注射化学发光法测定氢溴酸加兰他敏和力可拉敏

目的建立一种简单快速测定氢溴酸加兰他敏和力可拉敏的流动注射化学发光方法。方法在碱性条件下,加兰他敏与力可拉敏对鲁米诺-铁氰化钾发光体系有明显的抑制作用,且抑制效果与药物浓度呈线性关系。据此,建立了氢溴酸加兰他敏和力可拉敏的流动注射化学发光分析方法,并采用单因素优化方法对可能的影响分析方法的因素进行了优化。结果在优化条件下,加兰他敏和力可拉敏的线性范围分别为5×10-3～10mg/L和5×10-2～10mg/L;检出限分别为0.53μg/L和2.60μg/L。结论流动注射化学发光方法可以用于氢溴酸加兰他敏和力可拉敏药物制剂和生物样品的含量分析。     

Flow-injection-enhanced chemiluminescence method for the determination of three β-blockers

Objective To develop a rapid, simple and sensitive chemiluminescence method for the determination of three β-blockers (bisoprolol, atenolol and propranolol). Methods The chemiluminescence of cerium (Ⅳ)-sulfite system was obviously sensitized by adding anyone of three β-blockers in acid media. A new chemiluminescence method was set up by combining with flow-injection technique and used to determine the three β-blockers. Results Good linear ranges were obtained at the concentrations of 2.0×10-7g/mL-4.0×10-5g/mL, 1.0×10-7g/mL-3.0×10-5g/mL and 7.0×10-7g/mL-1.0×10-5g/mL, respectively, with the detection limits of 5.0×10-8g/mL, 7.0×10-8g/mL and 5.0×10-8g/mL (S/N=3), respectively, and the relative standard deviations for 11 times consecutive injections of 1.0×10-6g/mL bisoprolol, atenolol and propranolol were 3.57%, 2.21% and 2.26%, respectively. Conclusion The developed method is sensitive, accurate, rapid and of low cost. And it can be applied to determine bisoprolol, atenolol and propranolol in pharmaceutical preparations.     

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。     

CE-ECL法同时测定复方磷酸可待因中三种成分的方法学研究

目的 建立毛细管电泳-电化学发光法分离并检测复方磷酸可待因中三种成分,磷酸可待因、马来酸溴苯那敏和盐酸麻黄碱含量的新方法.方法 基于碱性介质中,复方磷酸可待因溶液中三种主要成分对联吡啶钌在铂电极上的电化学发光信号的增敏作用,且增敏强度和药物浓度成线性关系,与毛细管电泳联用,建立了毛细管电泳-电化学发光法分离并检测其含量的新方法.结果 在优化的实验条件下,确定三种药物对照品的线性范围、线性方程和检出限.通过对浓度为1.0×10~(-5)kg/L的磷酸可待因、马来酸溴苯那敏和盐酸麻黄碱对照品进行12次平行测定,其ECL发光强度的RSD值分别为2.89%,3.76%,3.32%.结论 该方法可用于复方磷酸可待因口服溶液中三种主要成分的含量测定,待测样品中的基质不干扰测定,方法的回收率分别为100.4%,101.9%,99.8%(n=5).     

HPLC-ELSD法测定桔梗中3种桔梗皂苷的含量

目的 建立测定桔梗药材中桔梗皂苷D、D3、E含量的方法.方法 采用高效液相色谱-蒸发光激光闪射检测器(HPLC-ELSD)法,Hypersil C18柱(5 μm,4.6 mm×150 mm),以乙腈-水为流动相梯度洗脱,流速1.0 mL/min,ELSD漂移管温度113℃,载气(N2)流速3.0 L/min.结果 桔梗皂苷D、D3、E的线性范围分别为13.78～275.6μg/mL(r=0.999 5)、8.40～168.0μg/mL(r=0.999 7)、12.02～240.4μg/mL(r=0.999 6),平均回收率(n=5)为98.3%、99.4%和101.3%.结论 本法操作简便,结果准确可靠,可用于桔梗皂苷D、D3、E含量的测定.     

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.     

Chemiluminescence determination of melamine with Luminol-K3Fe（CN）6 system

A sensitive chemiluminescence（CL） method was developed for determining melamine in urine and plasma samples based on the fact that melamine can remarkably enhance the chemiluminescence of Luminol-K3 Fe（CN）6 system in alkaline medium. The determination con     

脂肪乳剂体外溶血性试验的分光光度法的建立

目的建立分光光度法测定脂肪乳剂类药物体外溶血性试验的方法。方法用无水乙醇-浓盐酸作为破乳剂,使脂肪乳剂破乳、澄清,用分光光度法测定血红素在破乳环境下的吸光度。结果破乳剂中血红素的最大吸收波长在400 nm处。破乳剂与脂肪乳稀释液以16∶1(V/V)混合时,其吸光度(A)值为0.003±0.007。定量的血红素A值随破乳剂中盐酸浓度的减小而增大,当无水乙醇-浓盐酸为399∶1(V/V)时,其A值趋于稳定。16倍破乳剂无水乙醇-浓盐酸(399∶1)能充分破坏脂肪乳,使乳状液澄清,A值为0.002±0.001;该破乳条件下,溶血率在4%~100%时,溶血率-A值曲线的线性方程为Y=0.015X+0.03,r=0.999 6。结论脂肪乳剂加入16倍的破乳剂无水乙醇-浓盐酸(399∶1),使脂肪乳乳浊液澄清,可在400 nm波长处用分光光度法测定血红素的A值,判断溶血性。方法简便,可靠。     

Chemiluminescence enzyme immunoassay based on magnetic nanoparticles for detection of hepatoceUular carcinoma marker glypican-3

Glypican-3 （GPC3） is reported as a great promising tumor marker for hepatocellular carcinoma （HCC） diagnosis. Highly sensitive and accurate analysis of serum GPC3 （sGPC3）, in combination with or instead of traditional HCC marker alpha-fetoprotein （AFP）, is essential for early diagnosis of I-ICC. Biomaterial-functionalized magnetic particles have been utilized as solid supports with good biological compatibility for sensitive immunoassay. Here, the magnetic nanoparticles （MnPs） and magnetic microparticles （MmPs） with carboxyl groups were further modified with streptavidin, and applied for the development of chemiluminescence enzyme immunoassay （CLEIA）. After comparing between MnPs- and MmPs-based CLEIA, MnPs-based CLEIA was proved to be a better method with less assay time, greater sensitivity, better linearity and longer chemiluminescence platform. MnPs-based CLEIA was applied for detection of sGPC3 in normal liver, hepatocirrhosis, secondary liver cancer and HCC serum samples. The results indicated that sGPC3 was effective in diagnosis of HCC with high performance.     

Simultaneous determination of captopril and hydrochlorothiazide by time-resolved chemiluminescence with artificial neura

The combined use of chemometrics and chemiluminescence（CL）measurements,with the aid of the stopped-flow mixing technique,developed a simple time-resolved CL method for the simultaneous determination of captopril（CPL）and hydrochlorothiazide（HCT）.The stoppe     

NEW THERAPY FOR PUBIC SYMPHYSIS SEPARATION

ＮＥＷＴＨＥＲＡＰＹＦＯＲＰＵＢＩＣＳＹＭＰＨＹＳＩＳＳＥＰＡＲＡＴＩＯＮ（苟文丽），（屈新中），（赵正航）ＧｏｕＷｅｎｌｉ；ＱｕＸｉｎｚｈｏｎｇ；ＺｈａｏＺｈｅｎｇｈａｎｇ；（ＤｅｐａｔｍｅｎｔｏｆＧｙｎｅｃｏｌｏｇｙａｎｄＯｂｓｔｅｌｒｉｃｓ，Ｆ...