Determination of morphine in process streams by sequential injection analysis with chemiluminescence detection

A procedure for the determination of morphine in process streams by sequential injection analysis based on the chemiluminescence reaction of morphine with acidic potassium permanganate in the presence of sodium hexametaphosphate is presented. The chemiluminescence emission has been monitored using an in-house detection system which consisted of a fibre optic flowthrough cell and a sensitive, low dark current, photomultiplier tube. The calibration graph (range 2 × 10^–8 to 1 × 10^–4 mol/l) was not linear over the entire range of concentration, with a polynomial equation of best fit of y = 1.0 × 10¹⁵ x³ – 2.2 × 10¹¹ x² + 1.3 × 10⁷ x – 8.3. The calibration function approximates linearity over the concentration range 2.5 × 10^–6 to 3.0 × 10^–5 mol/l where the slope of the log-log plot is 1.09 ± 0.16. The detection limit was estimated at about 10^–8 mol/l from the response of the lowest calibration standard (2.5 × 10^–8 mol/l) which gave a signal to noise ratio of 3 : 1. Although the structurally related codeine did not interfere significantly the results suggest that this method may be susceptible to matrix effects, dependent on the location of sampling from the process stream.     

顺序注射化学发光联用技术测定空气中的SO2

基于在酸性溶液中SO32-被Ce4 氧化成SO42-产生很强的化学发光的原理,将顺序注射(SI)进样和化学发光(CL)检测方法联用,以0.012%三乙醇胺作吸收液,成功地测定了空气中的SO2。其浓度与发光信号强度在6.40×10-9～1.28×10-5mol/L范围内呈线性关系。方法的检出限(3σ)为4.80×10-9mol/L,对3.20×10-7mol/L的SO32-溶液9次测定的相对标准偏差为2.9%,方法回收率为98.45～103.6%。分析频率为90样/h。     

顺序注射化学发光联用技术测定食品中的碘

基于酸性溶液中HCHO存在下,KMnO4可氧化I-产生很强的化学发光的原理,建立了一个简单快速测定微量碘的顺序注射化学发光分析方法。I-在3.0×10-8~8.0×10-6mol/L范围内与发光强度呈良好线性关系。对2.0×10-6mol/L I-11次重复测定的相对标准偏差(RSD)为2.6%,方法的检出限(3σ)1.3×10-8mol/L,测定了4种食品中的碘量,回收率为92.8%~107.7%。分析频率为70 h。     

Determination of procaine, benzocaine and tetracaine by sequential injection analysis with permanganate-induced chemiluminescence detection

Local anaesthetics procaine hydrochloride (I), benzocaine (II), and tetracaine hydrochloride (III) were determined by the technique of sequential injection analysis (SIA) with chemiluminescence (CL) detection. The CL was emitted during the oxidation of the analytes by permanganate in aqueous sulphuric acid in the presence of various CL enhancers (4-hydroxybiphenyl, Rhodamine B, glycolaldehyde, glutaraldehyde and formic acid). The optimum enhancer or reagent concentrations, order and volumes of the injected zones were: 0.37 M formic acid (40, 23 or 28 mul for I-III, respectively), sample (40 mul), 2.3 M H(2)SO(4) (20, 16 or 18 mul for I-III, respectively), and 0.5 mM KMnO(4) (19, 13 or 15 mul for I-III, respectively). After a double (or single for III) reversal of the flow the mixed zone was pushed into the detector at a flow rate of 100 mul s(-1). The transient CL signal was recorded at >/=390 nm. The calibration graphs relating the intensity of the emission (peak heights) to the concentration of the analytes were curvilinear (a second order polynomial showed the best fit) and they were suitable for determining I-III in the ranges 0.5-50, 0.5-25 and 0.2-25 mug ml(-1), respectively. The limits of detection (3sigma) were 0.3 mug ml(-1) for I and II and 0.1 mug ml(-1) for III. The sample throughput was 120 h(-1). The relative standard deviations were 相似文献   

顺序注射化学发光法测定药物中的抗坏血酸

基于在酸性介质中KMnO4氧化抗坏血酸产生化学发光反应,HCHO的存在能使发光强度增强的原理,建立了顺序注射技术与化学发光分析联用测定痕量抗坏血酸的新方法。对进样顺序、体积、流速和浓度各因素进行了优化,在150μL进样体积下,方法的线性范围为1.0×10-9~2.0×10-6mol/L,检出限(3σ)为5.0×10-10mol/L,方法的相对标准偏差为1.3%(1.0×10-7mol/L,n=11)。采样频率为80样/h。应用该法测定维生素C针剂和片剂中的抗坏血酸,结果与标准方法一致。     

流动注射-化学发光法测定非洛地平

基于非洛地平在碱性条件下对鲁米诺-K3Fe(CN)6化学发光体系具有很强的增敏作用,结合流动注射技术,建立了直接测定非洛地平的流动注射-化学发光新方法.方法的线性范围为6.0×10(-9)～3.0×10(-6)g/mL,检出限为2.1×10(-9)g/mL,对浓度为1.0×10(-7)g/mL非洛地平平行测定11次,其...     

流动注射化学发光法测定盐酸美司坦

在碱性介质中,当把鲁米诺和KMnO4的混合溶液注入到盐酸美司坦溶液中时,会产生很强的化学发光现象。由此结合流动注射技术,建立了测定盐酸美司坦的流动注射化学发光新方法。该法的线性范围为2.0×10^-7-8.0×10^-6g/mL,检出限（3σ）为9×10^-8g/mL,对2.0×10^-6g/mL盐酸美司坦样品连续进行11次平行测定,其RSD为0.74%。已用于盐酸美司坦片剂中盐酸美司坦的测定。     

Determination of phenylephrine hydrochloride by flow injection analysis with chemiluminescence detection

A new method is proposed for the determination of phenylephrine hydrochloride by flow injection analysis with direct chemiluminescence detection. The method is based on the oxidation of the drug by potassium permanganate in sulfuric acid medium at 80 degrees C. The calibration graph is linear over the range 0.03-8 ppm phenylephrine hydrochloride, with a relative standard deviation (n = 51, 0.5 ppm) of 1.1% and sample throughput of 134/h. The influence of 38 different foreign compounds was tested, and the method was applied to the determination of phenylephrine hydrochloride in 8 different pharmaceutical formulations.     

流动注射-化学发光法测定富马酸依美斯汀

在酸性条件下,KMnO4与甲醛能够产生微弱的化学发光,而富马酸依美斯汀的存在能够大大增强该化学发光强度;结合流动注射技术,建立了测定富马酸依美斯汀的流动注射-化学发光新方法。该方法的线性范围分别为3.0×10-8～2.0×10-7g/mL,2.0×10-7～1.0×10-6g/mL和1.0×10-6～8.0×10-6g/mL。检出限为1.0×10-8g/mL,对2.0×10-6g/mL富马酸依美斯汀滴眼液平行测定11次,其相对标准偏差为1.3%。该方法已成功应用于滴眼液中富马酸依美斯汀的含量测定。     

Determination of sulphuric acid in process effluent streams using sequential injection titration

Sulphuric acid in process effluent streams from an electrorefining copper plant was analysed with a sequential injection (SI) titration system using sodium hydroxide as titrant. In the proposed SI titration system a base titrant, acid analyte and base titrant zone were injected sequentially into a distilled water carrier stream in a holding coil and swept by flow reversal through a reaction coil to the detector. The base zones contained bromothymol blue as indicator and the endpoint was monitored spectrophotometrically at 620 nm. The influence of carrier stream flow rate, acid and base zone volumes and titrant concentration on the linear range of the method was studied to obtain an optimum. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 0.006-0.178 mol l(-1) of H(2)SO(4) for a NaOH concentration of 0.002 mol l(-1). The results obtained for the SI titration of process samples were in good agreement with a standard potentiometric method with an RSD<0.75% and a sample frequency of 23 samples h(-1).     

流动注射化学发光法测定青霉素G钾

在甲醛的存在下,酸性KMnO4与青霉素G钾能够产生很强的化学发光,从而建立了KMnO4-甲醛-青霉素G钾化学发光体系来测定青霉素G钾.青霉素G钾的测定线性范围为2.0×10-7～1.0×10-5 g/mL,方法的检出限为1.4×10-7 g/mL,对4.0×10-7 g/mL的青霉素G钾进行11次平行测定,相对标准偏差为1.0%,用此法测定青霉素G钾取得了较好的结果.     

Determination of tetracycline by flow injection with chemiluminescence detection

Tetracycline hydrochloride (4 × 10^?5?1 × 10^?3M) in a 40-μl aqueous sample is determined in a flow system by measurement of the chemiluminescence emitted on reaction with bromine (9.3 × 10^?3 M) at pH 10.4 (carbonate buffer). The limit of detection is 1.6 nmol per 40-μl injection.     

精氨酸的流动注射化学发光法测定

在碱性介质中,精氨酸对硫氰化钾 鲁米诺化学发光体系有增敏作用,建立了用硫氰化钾 鲁米诺 精氨酸体系测定精氨酸的新方法。用该方法测定精氨酸的线性范围为0.01～2.0μg/mL,检出限0.01μg/mL,采样频率为190次/h,对3μg/mL的精氨酸连续平行测量10次,RSD为1.2%。用该方法对皮革屑中酶法提取的精氨酸进行了测定,并与氨基酸测定仪测定的结果进行了比较。     

顺序注射在线稀释测定人体液中尿酸

基于酸性条件下甲醛对尿酸-KMnO4发光反应的增敏作用,建立了在线稀释顺序注射化学发光联用技术测定人体液中尿酸的新方法。在选定的实验条件下的7个浓度梯度范围内,尿酸浓度在5.0×10-6mol/L~1.0×10-3mol/L范围内与发光强度呈良好线性关系,相关系数0.9942~0.9998,RSD在2.0%~3.5%之间,回收率为98.0%~103.0%。每小时可分析80个样品,在线稀释测定结果与手工稀释法一致。     

A screening test for heroin based on sequential injection analysis with dual-reagent chemiluminescence detection

A sequential injection analysis procedure with dual-reagent chemiluminescence detection was applied to the screening of street drug seizure samples for the presence of heroin. The chemiluminescence reagents (acidic potassium permanganate and tris(2,2'-bipyridine)ruthenium(III)) were aspirated from either side of a sample aliquot that was sufficiently large to prevent interdispersion of the reagent zones, and therefore two different chemical reactions could be performed simultaneously at either end of the sample zone. The presence of heroin in seizure samples was indicated by a strong response with the tris(2,2'-bipyridine)ruthenium(III) reagent and confirmed by a significant increase in the response with the permanganate reagent when the sample was treated with sodium hydroxide to hydrolyse the heroin to morphine. Nicomorphine (a morphine-derived pharmaceutical) was synthesised and tested under the same conditions. The responses with the permanganate reagent were similar to those for heroin, which supports the proposed chemical basis for the test. However, the responses with tris(2,2'-bipyridine)ruthenium(III) were far lower for nicomorphine than heroin (approximately 5-fold for the samples that had not been hydrolysed).     

Determination of carbaryl by flow injection with luminol chemiluminescence inhibition detection

A flow-injection procedure is described for the determination of carbaryl based on its inhibition effect on luminol-cobalt(II) chemiluminescence reaction in alkaline medium in the presence of hydrogen peroxide. The calibration data over the range 5.0?×?10^?7 to 20?×?10^?6?M give a correlation coefficient (r ²) of 0.9972 with relative standard deviations (RSD; n?=?4) in the range of 1.0–2.1% with a limit of detection (3?×?blank noise) of 2.37?×?10^?7?M for carbaryl. The sample throughput was 120?h^?1. The effects of some carbamates, anions, and cations were studied on luminol CL system for carbaryl determination. The proposed method has been applied to determine carbaryl in natural waters.     

流动注射化学发光法测定茶饮料中的茶多酚

在碱性条件下,茶多酚对鲁米诺-KMnO4化学发光体系具有较强的抑制作用,据此建立了茶多酚的流动注射化学发光测定法。该法的化学发光抑制值ΔICL与茶多酚质量浓度在2.0×10-6~5.0×10-4mg/mL范围内,呈现出良好的线性关系,检出限为1.2×10-7mg/mL,对1.0×10-5mg/mL茶多酚测定的相对标准偏差为2.9%(n=11)。用于茶饮料中茶多酚的测定。     

流动注射化学发光法测定DL-酪氨酸

在甲醛存在下 ,高锰酸钾与DL 酪氨酸能够发生化学发光反应 ,产生很强的化学发光。据此采用流动注射技术 ,建立了一种测定DL 酪氨酸的化学发光分析法。方法的检出限为 2 .9× 1 0 - 8g/mL ,相对标准偏差为 1 .5 % ( 1 .0× 1 0 - 6g/mLDL 酪氨酸 ,n =1 1 ) ,线性范围为 1 .0× 1 0 - 7g/mL～ 5 .0× 1 0 - 6g/mL。