不去蛋白直接光度法测定血清锌

建立了一种在表面面活性剂Brij-35存在下,用2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)作显色剂不去蛋白直接光度法测定血清锌的新方法.用该法测定血清锌,显色络合物最大吸收波长为560nm,线性范围0～46.0μmol.L-1,表观摩尔吸光系数为1.08×105L.mol-1cm-1,回收率为97.5%～102.8%,批内变异系数(CV)和批间变异系数分别为2.3%与3.7%.与原子吸收分光光度法比较具有良好的相关性.回归方程为y=1.01x-0.26,r=0.9884,P＞0.05.4例健康人血清锌含量为9.5～24.7μmol.L-1(x-±2S).用该法进行血清锌测定,准确性和重现性均较好,且血清用量少,不必去蛋白,操作步骤简化,具有快速、简便、灵敏可靠等优点,适合临床应用.     

改良的5-Br-PADAP光度法测定水中铜离子含量

目的建立了改良的5-Br-PADAP光度法测定水中铜离子含量。方法为在表面活性剂存在下,用2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)为显色剂测定水中铜离子含量。结果该法线性范围0~0.24 mg/L,平均回收率为99.9%,批内变异系数(CV)和批间变异系数分别为1.08%~2.62%和4.23%~4.57%,与原子吸收分光光度法比较具有良好的相关性,线性回归方程和相关系数分别为y=0.983 4 x+0.002 1,r=0.999 1。结论用改良的5-Br-PADAP光度法测定水中铜离子浓度方法简便、灵敏可靠,适合推广应用。     

5-Br-PADCAP分光光度法测定血清锌

为建立快速、简便、灵敏的分光光度法测定血清锌 ,在表面活性剂TritonX -1 0 0存在下 ,用 2 -(5 -溴 -2 -吡啶偶氮 ) -5 -[N ,N -二羧基甲基 ]苯酚 (5 -Br-PADCAP)作显色剂 ,不去蛋白分光光度法测定血清锌。结果表明 ,锌络合物最大吸收波长为 5 5 7nm ,线性范围 0～ 5 0 0μmol L ,摩尔吸光系数为 1 1 2× 1 0 5L·mol-1·cm-1。回收率为 99 9% ,批内变异系数 (CV)为2 1 % ,批间变异系数为 2 9% ,与原子吸收分光光度法 (x)比较具有良好的相关性 ,y =1 0 1 0x-0 1 5 4,r=0 991 8,P >0 0 5。可见本法测定血清锌不必去蛋白、用血量少、方法简便、灵敏可靠 ,适合临床应用     

三试剂自动分析法测定血清总铁结合力——5-Br-PADAP直接光度法

为建立简便、灵敏的测定血清总铁结合力(TIBC)自动化分析法,在表面活性剂存在下,用2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)为显色剂测定血清TIBC。该法线性范围0~180μmol/L,平均回收率为99.71%,批内变异系数(CV)和批间变异系数分别为0.024、0.041,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=0.994 3x 1.220 6,r=0.996 8。血清TIBC含量测定结果(-x±2s):105例健康男性48.0~76.0μmol/L,98例健康女性血清52.0~76.0μmol/L。可见用5-Br-PADAP三试剂自动化分析法测定血清TIBC方法简便、灵敏可靠,适合临床应用。     

以5-Br-PADAP为显色剂计算法测定血清总铁结合力

建立了以5-Br-PADAP为显色剂计算法测定血清总铁结合力(TIBC)的方法,通过测定血清铁和血清未饱和铁(UIBC)含量,以血清铁和血清UIBC含量之和计算血清TIBC含量。该法线性范围0~168μmol/L,平均回收率为100.4%,批内变异系数(CV)和批间变异系数分别为0.031、0.046,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=0.9978x 1.26,r=0.9745。65例健康男性血清TIBC含量为47.61~76.24μmol/L(x±2s),57例健康女性血清TIBC含量为52.56~77.45μmol/L(x±2s)。以5-Br-PADAP为显色剂计算法测定血清总铁结合力TIBC方法简便、灵敏可靠,适合临床应用。     

单一试剂光度法测定血清铜

建立了一种非离子型表面活性剂吐温 80 (Tween 80 )及聚乙二醇辛基苯基醚 (OP)存在下 ,用 2 ( 3 ,5 二溴 2 吡啶偶氮 ) 5 二甲氨基酚 ( 3 ,5 diBr DMPAP)作显色剂直接光度法测定血清铜含量的新方法。用该法测定血清铜 ,显色络合物最大吸收波长为 5 74nm ,线性范围达 63 0μmol·L- 1,表观摩尔吸光系数为 6 91× 1 0 4 L·mol- 1·cm- 1。回收率为 97 2 %～ 1 0 1 5 % ,批内和批间变异系数 (CV)分别为 2 7%与 3 8% ,与原子吸收分光光度法比较相关性良好 ,y =0 98x +0 43 ,r=0 9993 ,P >0 0 5 ,42例健康人血清铜含量为 8 3～ 2 4 9μmol·L- 1( x± 2s)。用该法进行血清铜含量测定 ,准确性和重现性均较好 ,且血清用量少 ,不必去蛋白 ,操作步骤简化 ,具有试剂单一稳定 ,操作简便快速 ,结果灵敏可靠等优点 ,适合临床应用。     

干法灰化-铬天青S光度法测定血清铝含量

建立了一种快速、灵敏测定血清铝的分光光度方法。血清标本经灰化处理后 ,在表面活性剂CPC存在下 ,用铬天青S (CAS)作显色剂测定血清铝 ,线性范围 0～ 7 4μmol/L ,平均回收率为 1 0 0 6% ,批内变异系数 (CV)和批间变异系数分别为 0 0 2 8和 0 0 3 7,与Al-CAS络合法比较具有良好的相关性 ,y =0 .990 2x -0 0 1 3 0 ,r =0 .9977,P >0 0 5。 42例健康人血清铝含量为 0 92～ 4 1 6μmol/L ( x± 2s)。用本法测定血清铝方法简便、灵敏可靠 ,适合临床应用。     

浊点萃取分光光度法测定水样中的痕量锌(Ⅱ)

为建立浊点萃取预富集测定水样中痕量锌的新方法,在表面活性剂TritonX-114存在下,利用5-Br-PADAP与锌(Ⅱ)产生显色反应的性能,采用分光光度法测定了水样中的痕量锌。结果表明,在pH8.5的NH3-NH4Cl缓冲体系中,锌(Ⅱ)与5-Br-PADAP形成紫红配合物,其最大吸收波长为λ=555 nm,摩尔吸光系数为ε=1.284×105L.mol-1.cm-1,检测限为0.003 7μg.mL-1.锌含量在0~1.2μg.mL-1范围内服从比尔定律。该法有较好的选择性,具有低毒、高效、安全、简便等特点,直接用于水样中痕量锌的测定,结果满意,重复6次测定相对标准偏差为2.18%。     

新的铬天青B直接光度法测定血清总铁结合力

为建立新的铬天青B直接光度法测定血清总铁结合力（TIBC）,在表面活性剂存在下,用铬天青B（CAB）为显色剂测定了血TIBC。结果表明,该法线性范围0～160μmol／L,平均回收率为99．4％,批内变异系数（CV）和批间变异系数分别为0．020、0．035,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=1．0033x＋0．4510,r=0．9982;60例健康男性血清TIBC含量为46．2～75．8μmol／L（x±2s）,60例健康女性血清TIBC含量为51．8～76．9μmol／L（x±2s）。用新的铬天青B直接光度法测定血清总铁结合力方法简便、灵敏可靠,适合临床应用。     

分光光度法测定精液锌的含量

建立了一种表面活性剂TritonX -1 0 0存在下 ,用 2 -(5 -溴 -2 -吡啶偶氮 ) -5 -二甲氨基酚 (简称 5 -Br-DMPAP)作显色剂直接光度法测定精液锌含量的新方法。该法显色络合物最大吸收波长为 5 5 6nm ,线性范围达 4 5 9mmol·L- 1,表观摩尔吸光系数为 1 1 2× 1 0 5L·mol- 1·cm- 1,回收率为 97 3 %～ 1 0 4 2 % ,批内和批间变异系数 (CV)分别为 3 1 %与 4 2 % ,与原子吸收分光光度法比较相关良好 ,y =0 984x +0 0 1 ,x =0 9869,P >0 0 5 (n =3 2 )。该法具有操作快速、简便、结果灵敏可靠等优点 ,适合在临床上推广应用     

二硫苏糖醇直接光度法测定钴离子含量

为建立简便、灵敏测定钴离子含量的方法,在表面活性剂存在下,用二硫苏糖醇(DTT)为显色剂测定钴离子.结果表明,该法线性范围0～6.00 mmol/L,平均回收率为99.4%,批内变异系数(CV)和批间变异系数分别为0.022、0.038,与原子吸收法比较具有良好的相关性,线性回归方程和相关系数分别为y =0.997 6...     

Spectrophotometric study of the reaction of zinc with O-hydroxybenzenediazoaminoazobenzene and its application

A highly sensitive and selective procedure for spectrophotometric determination of zinc has been developed. At pH 10.6, in the presence of emulsifier p-octylpolyethyleneglycol phenylether (OP), zinc forms an orange-red complex with o-hydroxybenzenediazoaminoazobenzene (HDAA) which has an absorption maximum at 525 nm. The molar absorptivity is 1.50 x 10(5) 1.mole(-1).cm(-1). Beer's law is obeyed for zinc in the range 0-13 mug/25 ml. The method has been applied to the spectrophotometric determination of trace amounts of zinc in aluminium alloy and in human hair. The proposed method is simple, rapid and accurate. No heating or separation is required.     

以金属离子为增稳剂的酶法终点法测定MPT- NAG含量

建立了快速、简便、灵敏地测定MPT - NAG含量的酶法终点法.以金属离子为增稳剂,N-乙酰-β-D-氨基葡萄糖苷酶(NAG)催化6-甲基-2-硫代吡啶-N-乙酰-β-D-氨基葡萄糖苷(MPT - NAG)水解,生成产物6-甲基-2巯基吡啶(MPT),MPT在340 nm处有吸收峰,通过测定340 nm处吸光度值计算M...     

Fluorimetric study of the interaction between human serum albumin and quinolones-terbium complex and its application

A highly sensitive spectrofluorimetric method is proposed for determination of human serum albumin (HSA) and some quinolone drugs. Using quinolones-terbium (Tb3+) complex as a fluorescent probe, in the buffer solution of pH 7.8, HSA can remarkably enhance the fluorescence intensity of the quinolones-Tb3+ complex at 545 nm and the enhanced fluorescence intensity of Tb3+ ion is in proportion to the concentration of HSA and quinolone drugs. Optimum conditions for the determination of HSA were also investigated. The linear ranges and limits of detection are 8.0 x 10(-9) to 8.0 x 10(-8) mol L(-1), 4.20 x 10(-9) mol L(-1) (for HSA); 1.0 x 10(-6) to 4.0 x 10(-6) mol L(-1), 1.87 x 10(-8) mol L(-1) (for norfloxacin) and 1.0 x 10(-7) to 1.0 x 10(-6) mol L(-1), 4.82 x 10(-8) mol L(-1) (for enoxacine), respectively. This method is simple, practical and relatively free interference from coexisting substances, as well as much more sensitive than most of the existing assays.     

灵敏的单一溴酚蓝测定尿蛋白

在pH 3.0的柠檬酸-柠檬酸钠缓冲液中,用溴酚蓝作显色剂,建立了一种快速、简便、灵敏、稳定的测定尿蛋白的分光光度法。该法显色络合物的最大吸收波长为620 nm,线性范围0~4.0 g/L,批内变异系数为0.52%,批间变异系数为1.27%,日间变异系数为1.51%,回收率为98.0%~99.3%,与邻苯三酚红比较有良好相关性,回归方程为y=0.030 0.830x,相关系数为r=0.9798。     

锌(Ⅱ)-茜素紫络合物的极谱行为及应用

用线性扫描示波极谱法研究了锌 ( ) -茜素紫络合物的伏安行为 ,发现在含有 0 .1 mol/L KCl,p H=9.96的 Britton- Robinson缓冲溶液中锌 ( ) -茜素紫络合物产生一灵敏的极谱吸附波 ,其峰电位为 - 1 .2 7V( vs.SCE) ,峰电流与锌 ( )的浓度在 8× 1 0 - 8～ 2× 1 0 - 6 mol/L的范围内呈线性关系 ,检出限为 5× 1 0 - 8mol/L。研究了电极反应机理 ,并用建立的方法成功地测定了发样中的锌     

Sensitive flow-injection amperometric detection of iodide using Mn3+ and As3+.

A rapid, selective, and sensitive kinetic flow-injection method for iodide content determination with amperometric detection on a platinum electrode was developed. The method is based on the catalytic effect of iodide on the Mn3+ reaction with As3+ in the presence of sulfuric acid. The calibration curve was linear in the concentration range from 5.0 x 10(-7) to 1.0 x 10(-4) mol/L iodide. The limit of detection (LOD) was found to be 5.0 x 10(-9) mol/L iodide. The relative standard deviations (RSD) were 1.68% and 3.03% for 1.0 x 10(-3) mol/L standard and 1.0 x 10(-6) mol/L iodide solution (n = 6), respectively. The method has been successfully applied for determination of iodide in waters, table salts, fodder, organic substances and human blood sera. The results were compared with those obtained by a standard AOAC (Association of Official Analytical Chemists) method, as well as with those obtained by a kinetic spectrophotometric procedure for determination of iodide.     

Amperometric detection studies of Nafion/indium hexacyanoferrate film for the determination of electroinactive cations in ion chromatography

An amperometric detector based on the chemical modification of Nafion and indium (III) hexacyanoferrate (II, III) thin film (Nafion/In-CN-Fe) onto a glassy carbon (GC) electrode, was first successfully used for the determination of electroinactive cations (Li+, Na+, K+, Rb+, Cs+, NH4+) in single column ion chromatography (IC). A set of well-defined peaks of electroinactive cations was obtained. The detection limits of the cations are 8.9 x 10(-6) mol/L for Li+, 2.3 x 10(-6) mol/L for Na+, 5.2 x 10(-6) mol/L for K+, 4.8 x 10(-6) mol/L for Rb+, 4.0 x 10(-6) mol/L for Cs+ and 5.3 x 10(-6) mol/L for NH4+ at a single-to-noise ratio of 3. The proposed method was quick, sensitive and simple. The cations in rainwater and mineral water were successfully analyzed by this method.     

Spectrofluorimetric determination of anthranilic acid derivatives based on terbium sensitized fluorescence.

Terbium sensitized fluorescence was used to develop a sensitive and simple spectrofluorimetric method for the determination of the anthranilic acid derivatives furosemide and mefenamic and tolfenamic acids. The method makes use of radiative energy transfer from anthranilates to terbium ions in alkaline methanolic solutions. Optimum conditions for the formation of the anthranilate-Tb3+ complexes were investigated. Under optimized conditions, the detection limits are 6 x 10(-9), 1.4 x 10(-8) and 9.0 x 10(-9) mol l-1 for furosemide, mefenamic acids and tolfenamic acid, respectively. The range of application is 2.5 x 10(-8)-5.0 x 10(-5) mol l-1 for all three drugs. The method was successfully applied to the determination of furosemide and mefenamic and tolfenamic acids in serum after extraction of the samples with ethyl acetate, evaporation of the organic layer under a stream of nitrogen at 40 degrees C and reconstitution of the residue with alkaline methanolic terbium solution prior to instrumental measurement. The mean recoveries from serum samples spiked with furosemide (5.0 x 10(-7), 2.0 x 10(-6) and 8.0 x 10(-6) mol l-1), mefenamic acid (3.0 x 10(-6), 9.0 x 10(-6) and 3.0 x 10(-5) mol l-1) and tolfenamic acid (3.1 x 10(-6), 12.5 x 10(-6) and 2.5 x 10(-5) mol l-1) were 96 +/- 8, 101 +/- 5 and 98 +/- 7%, respectively. The within-run precision (RSD) for the method for two serum samples of each drug varied from 2 to 8% and the day-to-day precision for two concentration levels varied from 2 to 13%.     

Simple, sensitive and rapid liquid chromatographic/electrospray ionization tandem mass spectrometric method for the quantification of lacidipine in human plasma

A simple, sensitive and rapid liquid chromatographic/electrospray ionization tandem mass spectrometric method was developed and validated for the quantification of lacidipine in human plasma using its structural analogue, amlodipine, as internal standard (IS). The method involves a simple single-step liquid-liquid extraction with tert-butyl methyl ether. The analyte was chromatographed on an Xterra MS C(18) reversed-phase chromatographic column by isocratic elution with 20 mM ammonium acetate buffer-acetonitrile (10:90, v/v; pH 6) and analyzed by mass spectrometry in the multiple reaction monitoring mode. The precursor to product ion transitions of m/z 456.4 --> 354.4 and m/z 409.3 --> 238.3 were used to measure the analyte and the I.S., respectively. The chromatographic run time was 1.5 min and the weighted (1/x(2)) calibration curves were linear over the range 0.1-25 ng ml(-1). Lacidipine was sensitive to temperature in addition to light. The method was validated in terms of accuracy, precision, absolute recovery, freeze-thaw stability, bench-top stability and re-injection reproducibility. The limit of detection and lower limit of quantification in human plasma were 50 and 100 pg ml(-1), respectively. The within- and between-batch accuracy and precision were found to be well within acceptable limits (<15%). The analyte was stable after three freeze-thaw cycles (deviation <15%). The average absolute recoveries of lacidipine and amlodipine (IS) from spiked plasma samples were 51.1 +/- 1.3 and 50.3 +/- 4.9%, respectively. The assay method described here could be applied to study the pharmacokinetics of lacidipine.