N-溴代琥珀酰亚胺(NBS)-罗丹明B化学发光体系测定苯酚的研究

在碱性条件下苯酚可被N-溴代琥珀酰亚胺(NBS)氧化,其能量激发共存的荧光物质罗丹明B产生强烈发光。基于此现象,并结合流动注射分析技术,建立一种直接测定苯酚的流动注射化学发光分析方法。在最佳条件下,苯酚浓度在1.0×10-3mg/L~5.0×10-1mg/L范围内与发光强度呈线性关系(ΔI=334.1C 5.237,C:mg/L,r2=0.9985),检出限为5.7×10-4mg/L(3σ)。1.0×10-2mg/L苯酚9次平行测定,相对标准偏差(RSD)为2.7%。     

流动注射化学发光法测定兰索拉唑的研究

兰索拉唑在Ag NPs-Luminol-K3Fe(CN)6化学发光体系中能够产生强烈的化学发光信号,结合流动注射分析技术,提出了检测兰索拉唑的化学发光新方法。在实验条件下,本法测定兰索拉唑的线性范围为3.0×10-3~1.5 mg/L,检出限为2.0×10-4mg/L(3σ),相对标准偏差为1.5%(n=11,c=3.0×10-2mg/L)。方法用于片剂及人血清中兰索拉唑的含量测定,回收率为98.0%~102.5%。同时,对可能的化学发光反应机理进行了初步探讨。     

流动注射化学发光法测定氧雄龙

氧雄龙对Ce(Ⅳ)-SO32-体系的化学发光有较强的增敏作用,据此建立了氧雄龙的流动注射化学发光测定法.方法的线性范围和检出限分别为0.1～10 mg/L和4.8×10-3mg/L,相对标准偏差(n=11,c=1.0 mg/L)为3.3%.     

流动注射化学发光法测定曲克芦丁

基于曲克芦丁对Luminol-K_2S_2O_化学发光体系的强烈抑制作用,结合流动注射技术,建立了流动注射化学发光法测定曲克芦丁的新方法.在优化的实验条件下,该法的线性范围为1.0 ×10~(-7)～6.7×10~(-5)mol/L,检出限为8.0×10~(-8)mol/L,对4.0×10~(-7)mol/L曲克芦丁进...     

流动注射化学发光法测定3种氟喹诺酮类药物

研究发现,氟喹诺酮类药物对可溶性Mn(-甲醛化学发光体系有强烈的增敏作用,结合流动注射技术,建立了3种氟喹诺酮类药物诺氟沙星、氧氟沙星和环丙沙星的流动注射化学发光新方法。在优化的实验条件下(2×10-4molMn(-3%甲醛-3mol/L磷酸),本方法测定诺氟沙星、氧氟沙星和环丙沙星的线性范围分别为1.0×10-7～1.0×10-5mol/L,1.0×10-7～1.0×10-5mol/L和3.0×10-7～5.0×10-5mol/L;检出限分别为3×10-8mol/L,3×10-8mol/L,1×10-7mol/L;相对标准偏差(5.0×10-6mol/L氟喹诺酮类药物,n=11)分别为2.6%,1.6%和2.8%。该方法已用于诺氟沙星胶囊中诺氟沙星的含量测定。     

流动注射化学发光法测定大豆异黄酮

基于在NaOH碱性介质中,K3Fe(CN)6可以直接氧化大豆异黄酮产生强的化学发光这一现象,并结合流动注射分析技术,提出了直接化学发光测定大豆异黄酮含量的新方法。当K3Fe(CN)6浓度为5.0×10-4mol/L,NaOH浓度为0.5 mol/L,主副蠕动泵转数分别为45 r/m in和35 r/m in时,体系具有最强的化学发光。该方法测定大豆异黄酮的线性范围为1.0×10-3~0.5 g/L;其回归方程为A(峰面积)=193305C(mg/L) 229.97,r=0.9962;检出限为4.6×10-4g/L。对5.0×10-3g/L大豆异黄酮溶液连续测定,每次得3个峰值,重复7次,相对标准偏差为2.46%。本方法已用于大豆中异黄酮含量的测定。     

流动注射化学发光法测定呋塞米

在酸性条件下呋塞米对Ce(Ⅳ)-Na_2SO_3弱化学发光体系具有很强的增敏作用,据此建立了流动注射化学发光法测定呋塞米的新方法.该法测定呋塞米的线性范围为0.01～1.0 mg/L,检出限为4×10~(-3)mg/L(3σ),RSD为2.2%(n=11,ρ=0.2mg/L),回收率为95%～105%.该法已应用于片剂和针剂中呋塞米含量的测定.     

反相流动注射化学发光法测定甲硝唑

在硫酸介质中,高锰酸钾氧化鲁米诺产生化学发光,甲硝唑对该体系有一定的抑制作用。据此,建立了反相流动注射化学发光法测定甲硝唑的新方法。甲硝唑浓度在1.4×10-3~2.0×10-2mg/mL范围内,相对化学发光强度△I与甲硝唑含量的对数呈良好的线性关系;方法的检出限(3σ)为1.0×10-3mg/mL;相对标准偏差(c=0.02mg/mL,n=11)为1.8%。本法应用于片剂中甲硝唑含量的测定,结果满意。     

偶合反应流动注射化学发光法测定扑热息痛

基于扑热息痛还原铬(Ⅵ)和铬(Ⅲ)催化鲁米诺-过氧化氢的化学发光,建立了氧化还原偶合反应流动注射化学发光法测定扑热息痛的新方法.方法线性范围为4.0×10-9～4.0×10-5mol/L,检出限为1.0×10-9 mol/L.对4.0×10-7 mol/L扑热息痛平行测定8次,其标准偏差为2.7%.已将该方法用于片剂中...     

双[2,4,6-三氯苯基]草酸酯-过氧化氢体系流动注射化学发光法检测地沟油中的胆固醇

基于胆固醇和冰乙酸的反应物与硫酸铁铵生成的紫色化合物能有效抑制双[2,4,6-三氯苯基]草酸酯(Bis(2,4,6-trichlorophenyl)oxalate,TCPO)-H2O2-咪唑化学发光反应,建立了流动注射-化学发光联用检测胆固醇的方法。对流动注射、化学发光等实验参数进行了优化。当咪唑浓度为0.001 mol/L,H2O2浓度为0.3 mol/L,TCPO浓度为1.0×10"3mol/L,主副蠕动泵转数分别为20和15 r/min时,体系具有最强的化学发光。在优化的实验条件下,测定胆固醇的线性范围为8.6×10"6～2.2×10"4mol/L;检出限(S/N=3)为2.5×10"6mol/L;相对标准偏差(RSD,n=11,c=6.5×10"5mol/L)为1.5%。不同加标水平下的加标回收率为95.0%～105.0%;相对标准偏差(n=6)小于3.6%。本方法已应用于地沟油中胆固醇的测定,结果令人满意。     

流动注射化学发光法测定水样中痕量间苯二酚

基于在甲醛存在条件下,高锰酸钾在酸性介质中氧化间苯二酚而发生化学发光反应,建立了测定痕量的间苯二酚化学发光分析法.该法测定间苯二酚的线性范围为5.0×10-9～1.0×10-4mol/L,检出限为3.0×10-9mol/L,相对标准偏差为3.5%(1.0×10-6mol/L间苯二酚,n=11).该法应用于测定水样中加入的间苯二酚,结果令人满意.     

Luminol-K_3[Fe(CN)_6]流动注射化学发光体系检测头孢吡肟

在碱性介质中,头孢吡肟对Luminol-K3[Fe(CN)6]化学发光体系具有明显的增强作用,基于此建立了流动注射化学发光法测定头孢吡肟的新方法。在优化实验条件下,化学发光增强强度与头孢吡肟的浓度在3.0×10-6~4.0×10-5g/m L范围内呈良好的线性关系,检出限为2.8×10-6g/m L。对2.0×10-5g/m L头孢吡肟平行测定11次,相对标准偏差(RSD)为1.5%。该方法用于头孢吡肟针剂的测定,结果满意。     

流动注射后化学发光法测定异烟肼

本文发现了异烟肼在铁氰化钾-钙黄绿素化学发光反应体系中的后化学发光反应。优化了反应条件,建立了一种利用后化学发光反应测定异烟肼的流动注射化学发光分析法。方法的检出限为6×10-8g/mL, 相对标准偏差为1.8% (2.0×10-6 g/mL 异烟肼,n=11）,线性范围为2.0×10-7~1.0×10-5 g/mL。此法已用于异烟肼片剂中异烟肼含量的测定,结果与药典方法测定值一致。     

分子印迹-流动注射化学发光测定磺胺二甲基嘧啶

本文以二乙烯三胺为功能单体,环氧树脂为交联剂,磺胺二甲基嘧啶(SM2)为目标分子,合成了对SM2具有专一性识别的分子印迹聚合物(MIP)。在酸性条件下,利用HCl-KMnO_4-甲醛发光体系,结合流动注射化学发光(FI-CL),建立了测定SM2的MIP-FI-CL分析方法。方法的线性范围为1.0×10~(-4)~1.5×10~(-3) mol/L,检出限为6.0×10~(-5) mol/L。该方法可用于测定复杂样品中SM2的含量。     

Determination of Genistein by Flow‐injection Chemiluminescence Method Based on Ferricyanide Oxidation Sensitized by Rhodamine 6G

A novel flow injection chemiluminescence (FI‐CL) method for the determination of genistein was described. The method was based on the reaction between genistein and potassium ferricyanide in alkaline solution to give weak CL signal, which was dramatically enhanced by rhodamine 6G (Rh G). The CL emission allowed quantitation of genistein concentration in the range 1.0 × 10^?7–4.0 × 10^?5 mol/L with a detection limit (3σ) of 4.2 × 10^?8 mol/L. The relative standard deviation for 11 parallel measurements of 5.0 × 10^?7 mol/L, 4.0 × 10^?6 mol/L and 1.0 × 10^?5 mol/L genistein were 2.59%, 2.40% and 1.48%, respectively. The experimental conditions for the CL reaction were optimized and the possible reaction mechanism was discussed. The method was applied to the determination of genistein in biological fluids.     

Flow Injection Chemiluminescence Determination of Puerarin in Pharmaceutical Preparations Using Eosin Y‐Fenton System

A novel chemiluminescence (CL) system was established for the determination of puerarin in pharmaceutical preparations. It was shown that a strong CL signal was observed when Eosin Y reacted with the hydroxyl radicals which were generated from Fenton reagent in acidic medium. The CL intensity was decreased significantly when puerarin was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with puerarin concentration. Based on this, a new method for the determination of puerarin using a flow injection chemiluminescence technique was developed. The experimental parameters that affected the CL intensity were optimized. Under the optimal conditions, the linear range for puerarin concentration was 8.0×10^?8?2.0×10^?6 mol/L (R=0.9982) with a detection limit of 7.5×10^?9 mol/L (S/N=3) and the relative standard deviation was 1.7% for 4.0×10^?7 mol/L puerarin (n=11). The proposed method was applied to the determination of puerarin in a puerarin injection with satisfactory results.     

鲁米诺-过氧化氢化学发光体系测定利福平

基于鲁米诺在碱性条件下可以被H2O2氧化产生化学发光,利福平对此化学发光具有增敏作用这一现象,结合流动注射技术建立了一种直接测定利福平的流动注射化学发光新方法.该方法的线性范围在1.0×10-6～2.0×10-8g·mL-1,检出限为3.0×10-9g·mL-1,对5.0×10-7g·mL-1的利福平连续进行11次平行测定,其相对标准偏差为3.0%.该法已成功测定了利福平胶囊及眼药水中利福平的含量.     

Flow Injection Chemiluminescence Determination of Prednisone Acetate by Oxidation with N-Bromosuccinimide

A simple flow injection chemiluminescence (CL) method for the determination of prednisone acetate was developed. This method is based on the fact that the strong CL of N-bromosuccinimide (NBS) and calcein can be inhibited by prednisone acetate. The CL intensity correlated linearly with the concentration of prednisone acetate over the ranges of 0.02–0.4 mg/L and 0.4–10 mg/L. The CL mechanism was also proposed. The detection limit (3σ) of prednisone acetate was 13 ng/mL and the relative standard deviation was 1.3% at 0.1 mg/L prednisone acetate (n = 11 measurements). This method was applied to the determination of prednisone acetate in the tablets with good results.     

Determination of Diammonium Glycyrrhizinate and Its Antioxidant Activity Using a Novel Chemiluminescence System

A novel chemiluminescence (CL) system was established for the determination of diammonium glycyrrhizinate (DG) in pharmaceutical preparations and its ability of scavenging hydroxyl radical. It was shown that a strong CL signal was observed when Eosin Y mixed with Fenton reagent. The CL intensity was decreased significantly when DG was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with DG concentration. Based on this, we developed a new method for the determination of DG using a flow injection chemiluminescence (FI-CL) technique. Under the optimal conditions, the linear range of DG concentration was 6.0 × 10^?8–5.0 × 10^?6 mol/L (R = 0.9982) with a detection limit of 8.0 × 10^?9 mol/L (SN = 3), and the RSD was 3.8% for 2.0 × 10^?7 mol/L DG (n = 11). This method was successfully used in the determination of DG in tablets and the evaluation of hydroxyl radical scavenging capacity of DG. The possible reaction mechanism of the CL system is discussed.     

Flow Injection Chemiluminescence Determination of Phenol in Neutral Medium

A new flow injection chemiluminescence method for the determination of phenol was proposed, based upon the chemiluminescence reaction of phenol, N-bromosuccinimide, and hydrogen peroxide in neutral aqueous medium in the presence of cetyltrimethylammonium bromide surfactant micelles. The chemiluminescence signal was proportional to the concentration of phenol in the range of 1.0 × 10^?7?8.0 × 10^?6 g/mL with a detection limit of 3 × 10^?8 g/mL. The relative standard deviation for 1.0 × 10^?6 g/mL phenol solution was 2.0% (n = 11). The proposed method was successfully applied to the determination of phenol in phenol ear drops. A possible CL reaction mechanism was also discussed briefly.