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The Applications of Flow Injection Analysis Coupled with LuminolChemiluminescence in Basic Medium.

Byline: Attiq-Ur-Rehman Kakar, Naqeebullah Khan, Samiullah, Naeemullah Amir Waseem and Fazal Ur Rehman

Summary: Chemiluminescence has appealed significant attention in multidisciplinary diagnostic research fields and revealed various encouraging applications due to its unique selective and sensitive nature. This paper provides a comprehensive review about the principles of flow injection analysis (FIA) and the important parameters regarding the technique. The ideology of chemiluminescence (CL), luminol (Lu) as a CL reagent and its applications in basic medium (liquid-phase) when coupled with FIA as a diagnostic tool in diverse fields of analytical chemistry have been described. The data of 107 papers, which appeared in the literature from 2013 to present (up to our access) for the determination of vital analytes in diverse sample matrices in terms of chemical reaction, sample matrix, analyte, dynamic linear range, limits of detection, sample throughput and coefficient of determination is presented in the tables.

The reactions based on FILu-CL involved in mechanistic and chemical studies of medically important substances have also been reviewed. The use of nanotechnology has improved the analytical and diagnostic characteristics of FI-CL strategies by improving the detection limits and further advancements are expected in future with the discovery of new synthetic nano-particles.

Keywords: Flow injection, Dispersion, Chemiluminescence, Luminol, Nano-technology.

Introduction

Flow Injection Analysis It is the demand of present age to carry out trace, rapid, precise and accurate analysis with minimum budget in many fields like environmental, industrial, pharmaceutical, clinical and food analyses. A very useful technique i.e. flow injection analysis (FIA) fulfilling these demands and was first introduced by two Danish researchers Ruzicka and Hansen in 1975 [1]. One year later, the inventors proposed several practical techniques [2]. Eleven years later, the authors reported a widespread review about the new progresses made in FIA [3] that describes the wide range applications of FIA in the fields of chemical, biological, environmental and pharmaceutical analyses covering several books (39) and 13000 publications [4]. It is because, this technique allows analysts to easily automate and optimize powerful wet chemical methods for routine laboratory analyses.

Due to its small sample volume and reagent consumption, online matrix separation and/or pre-concentration phase with high sample throughput, it is widely accepted as a powerful tool for analytical procedures within the science world and numerous reviews and books have been published about its applications [5, 6].

Principle of FIA

The basic principle of FIA involves the introduction of liquid sample into a liquid constant sinuous stream known as sample transporter. The introduced sample becomes a part of moving incessantly carrier stream and produces a region, into which preset reagents at a definite flow rates are mixed. During flow in a mixing coil, chemical reaction takes place yielding analyte into a detectable substance. The processed sample mover is finally then conceded towards a detector that reports signal of electrode potential, absorbance, fluorescence or other physical property of the sample traveling through the flow cell of volume about 8 ul [7]. Finally, the sample is washed out.

FIA manifold

A simple manifold for FIA can be designed with the tools such as a pump (peristaltic), an injection valve (rotary), flexible plastic tubes to connect the injection valve, a flow through cell having small volume (up to 300 ul) and a suitable detection system (Fig. 1) [8]. A peristaltic pump (2-8 channels) takes the sample carrier and reagents from their reservoirs and propel them forward with a desired constant flow rate (0.5 to 3.0 ml/min).An injection valve (a six port) permitting the reproducible injection of a properly calculated size of sample (10 - 300 ul) into the sinuous flow with no cessations. A common syringe or a peristaltic pump could be used to fill the loop of the injection valve. The manifold is made up of flexible silicon/tygon tubings with consistent internal diameter (0.5-0.8mm). Reaction coils of any length could be incorporated in the manifold for the proper mixing of the reagents.

The flexibility of FIA about detection system is the main reason of its versatility. Nearly any flowthrough detector for drenched chemical reactions could be used in FIA, most common is UV/Visible spectrophotometry [9], chemiluminescence (CL) [5], electrochemiluminescence (ECL) [10] and others [11, 12]. Often, flow injection analysis is called as flow analysis or automatic analysis [13]. Several types of FIA have been designed in the last few decades which include reverse flow injection analysis (rFIA), merging zone analysis, flow batch analysis, sequential injection analysis (SIA), Lab on valve (LOV), bead injection analysis, multi-pump flow analysis (MPFA) etc [13]. For automated operations, computers may be applied to regulate the introduction of sample, injection valve, pump speed and detection system [14].

Dilution or Dispersion

In FIA system, the degree of dilution or dispersion is characterized by the dispersion coefficient (D), which is stated as, "the ratio of sample concentrations before and after the dispersion process takes place" [1] and is mathematically written as:

D = CAdeg/C

where CAdeg is the concentration of injected sample and C is the concentration of sample at the detector. Dispersion is affected by the factors such as tube length, tube diameter, sample volume and flow rate. The sample dispersal for simplicity, is termed as limited dispersion (D = 1-3), medium dispersion (D = 3-10) and large dispersion (D [greater than or equal to] 10), and the FI systems are made up of and thought-out consequently for several investigative applications [15].

Salient features

The flexibility of FIA has made it multipurpose analytical technique which fulfills the demands of researchers. The manifold for FIA can be designed as per need providing a compact, contamination free, speedy and reliable analytical systems that could be deployed in fields, resulting in situ analysis and good resolution monitoring, with great reproducibility (typical relative standard deviations (RSDs) of 1-5%), high number sample through put (20- 300 h -1), good precision (typically <2% RSD) and high accuracy [4]. In addition, FIA manifolds offer on-line sample pretreatment systems to remove matrix by incorporating solid phase column [14] and sample preconcentration [16] amazingly increasing the sensitivity and selectivity of the analytical procedures.

Chemiluminescence Reaction

Luminescence, from Latin word lumen (light) [17] is a production of photons in IR or UV/Visible region by an electronically excited species.CL is the emission of light during the progress of a reaction devoid of producing heat. A reactant specie during the course of reaction is excited and it releases light in returning to ground state (Fig. 2(a), direct CL) or if incompetent emitter then its energy might be transferred to a sensitizer for light emission (Fig. 2(b),indirect CL). In CL, the reaction provides energy to promote an intermediate to an excited state, along the consequent processes of vibrational repose, internal conversion and inter-system trip occur that permit the emission of light [8].

a) X + Y [I]*Products + h (direct CL)

b) X + Y [I]* + S S* Products + h (indirect CL)

Light measurement from a chemical reaction is of great importance and incredibly valuable from analytical point of view for the reason that under proper experimental circumstances, the light intensity produced is directly related to the analyte concentration, hence permitting sensitive and precise quantitative determinations. Compared with other analytical techniques like fluorimetry, resonance light scattering methods, spectro-photometry etc, and the main attractions of CL systems for analytical applications is their admirable sensitivity over a wide linear dynamic range, low detection limits and requiring no external excitation source so, the background signal is very low. The main drawback of CL reactions is the lack of selectivity which is because most of the CL reagents emit light with several analytes. This limited selectivity can be overcome by coupling with FIA which provides online physical separations [18].

The versatility of CL reactions for determination of a wide variety of analyte is due to their participation in CL reaction such as CL substrates or CL precursors accountable for the excited state, the essential reagent for the CL reaction (an oxidant usually); certain analytes that affect the efficiencies or rate of CL processes, activators such as catalyst (enzymes or metal ions) or quenchers such as reductants that quench the CL emission, fluorophores in the case of sensitized CL. Some analyte which do not directly take part in the CL process but can be coupled with other reagents to produce a specie which is a reactant in the CL reaction, species that can be derivatized with some CL precursors or fluorophores. Subject to the nature of the analyte and the CL process the enhancement or inhibition of CL intensity will be directly related to the analyte concentration [19].

Luminol Reaction

The most commonly used CL reagent is luminol (Lu) (5-amino-2,3-dihydro-1,4-phthalazinedione) and Schimtza German scientist in 1908 has often been suggested as the creator of luminol [20]. The CL of luminol oxidation (Fig. 3) in an aqueous alkaline medium (pH 10 - 11) generates excited aminophthalate ion [21]. This reaction has less quantum yield (a0.01) and the emission is bluish with its wavelength maximum around 425 nm [22]. Luminol CL reaction is produced in the presence of a range of catalysts, just about certain for a definite oxidizing species and variable efficacies. Usually an extracted enzyme known as horseradish peroxidases (HRP) the most efficient catalyst which undergoes at pH around 7 [23] and for a certain auxiliary-oxidants (e.g. ferrocene, ferricyanide) are used as catalysts with moderate efficiencies that are selective like hydrogen peroxide (H2O2).

Transition metal cations 2+ 3+ 2+ 2+ (Fe, Fe2+, Co2+, Cr4+, Cu2+, Hg, Mn, Ni) and their complexes associated to achieve comparatively lesser signal to noise ratios with high reactions pH [24]. Both the enhancement and inhibition of the reactions have considerable attraction for analysts and find numerous applications in the field of analytical chemistry. Applications of enhancement and inhibition of FI-Lu-CL reactions

Enhancement of FI-Lu-CL reaction in the presence of different oxidants

The light emission during Lu-CL reaction can be enhanced by a wide range of analytes in diverse sample matrices using different metals and oxidants (Table 1.1). Transition metals are the good catalysts for Lu-CL reactions. In the presence of dissolved oxygen Lu-FI-CL reaction has been used for the detection of cadmium [25], fentanyl citrate [26] and pesticides [27].

The most useful oxidant, H2O2 has been widely used in Lu-CL reaction for the determination of iron(II) (using poly acrylic acid gel beads for immobilization) [28], iron(III) [29], chromium (III) (using a gravity and capillary force driven flow) [30], iron(II) and H2O2 [31], creatinine (using cobalt as catalyst) [32], bovine serum albumin [33], amino acids like histidine and lysine [34] and tryptophan (with firefly-liquid waveguide-flow cell) [35], sarafloxacin [36], vitamin A and C and rose bengal (using copper(II) catalyst) [37], organic peroxides by acid degradation to yield H2O2 (using copper(II) as catalyst) [38] and glycated emoglobin (using modified gold substrate) [39].

Mingxia et al. used HRP for the analysis of salbutamol by immobilizing coating-antigen on beads of carboxylic resin and introducing the second antibody tagged with HRP into Lu-p-iodophenol(PIP)-H2O2-CL reaction [40]. Unpolluted river water to raw sewage samples were analyzed using Lu-H2O2 in good limits 41]. Similarly, human prealbumin was determined by the same reaction after immobilizing onto functionalized magnetic beads [42]. The reaction of Lu with potassium ferricyanide (K3Fe(CN)6) has been used for the detection of mezlocillin sodium [43] and ceftezole sodium [44] whereas, with periodate(IO4) for amikacin sulfate [45] and vitamin A [46] and with potassium permanganate (KMnO4) for fenpyroximate [47], azoxystrobin [48] and thyroxine (in micellar medium) [49].

The oxidation of Lu can be achieved with several other reagents and used for quantification like 5-sulfosalicylic acid for platinum [50], diperiodatocuprate(III) for ractopamine [51], bovine serum albumin for formaldehyde [52], hydrazine for hemoglobin [53], urea peroxide for 2,20-([1,10-biphenyl]-4,40-diyldi-2,1-ethenediyl)bisbenzenesulfonic acid disodium salt [54], Nbromosuccinimide for phenols (using solid-liquid extraction) [55] and perborate/percarbonate for copper(II) (using ion exchange chromatography for separation) [56]. In some reactions the analytes like benzoyl peroxide [57] and isoamyl nitrite [58] oxidize the CL reagent.

Enhancement of FI-Lu-CL reaction in the presence of nanomaterials

Nanomaterials like nanoparticles (NPs), nanocluster or nanocompsites (NCs), quantum dots (QTs), carbon dots (CDs) and graphene or graphene oxides (GQTs) have been widely employed in CL reactions due to their special structure, large surface area and properties which improve quantum efficiency, selectivity, sensitivity and accuracy (Table-1.2). Several reviews have been published on the recent advances in the CL reactions based on nanomaterials and applications in the analytical analyses [59]. Gold nanoparticles (Au-NPs) due to their easy preparation and large surface to volume ratio have been largely used in the CL reactions as a catalyst for analytical purposes. Based on the enhancement of Lu-CL-reactions with H2O2, Au-NPs strategies have been developed for detection of several analytes like manganese(II) [60], human immunoglobin G (functionalized Au-NPs with high ratio of HRP) [61] and with K3Fe(CN)6 for ascorbic acid [62].

The antibiotic, chloramphenicol has been detected using the same CL reaction by Lu functionalized silver NPs for the labeling of the analyte [63]. Alpha-fetoprotein was determined after labeling by iron based metal organic framework (MOFs) [64]. Iron oxide magnetic NPs capped with oleic acid have been used for hydroquinone determination [65]. Zinc oxide NPs have been used for the detection of H2O2 [66]. A high throughput method for serum uric acid (SUA) detection based on the production of H2O2 by SUA and immobilized uricase and the CL reaction was catalyzed by mesoporous metal oxide NPs [67]. Microcystin-LR has been determined using magnetic beads modified (MMB) with polyethyleneimine and immobilized anti-micocystin-LR that capture the microcystin-LR in water which react with HRP co-immobilzed silica NPs. [68]. Cobalt-iron layered double hydroxides (Co-Fe-LDH) NPs also showed enhancement of Lu-H2O2-CL reaction and was used for H2O2 and glucose detection [69].

The Lu-IO3 CL reaction in the presence of cobalt could be enhanced by silver NPs and has been used for pyrogallic acid determination [70]. Nanosheets as enhancer of the CL reactions have also been reported [71, 72]. Copper oxide nanosheets were synthesized sonochemically which were employed as enhancer in the CL reaction of Lu-KMnO4 for meropenem [71] and Lu-H2O2 for cloxacillin determinations [72]. Graphene which is one-atom-thick planar sheet of sp2-bonded carbon atoms owning the advantages of large surface area, high conductivity, low production cost and enhancement of CL reactions. A functional material was synthesized by graphene nanosheets supporting Pt-Co bimetallic nanodendrite hybrid showing high catalytic activity to Lu-H2O2-CL reaction and was used for glucose detection [77] and chitosan modified magnetic oxide grapheme (MGO) composite for thrombin detection [78].

For the determination of lysozyme, surface molecularity imprinted polymers of MGO multi-walled carbon nanotubes (MWC-NTs) were prepared which enhance Lu-H2O2-CL reaction [79].Metal-organic gels (MOGs) are metal-organic hybrid materials synthesized by gathering organic ligands and metal ions through metal ligand coordination and noncovalent interactions owning easy availability with low-cost and non-toxic nature, greatly enhance Lu-CL reactions. Dopamine has been determined using iron(III) a central metal with ligand 1,10-phenanthroline-2,9-dicarboxylic acid-MOG [80] and cysteine using cobalt(II) metal-organic framework from (Zn-MOGs) [81]. Semicoductor QTs with unique electronic and optical properties are inorganic materials that enhance CL reactions [73-76]. The enhancement of Lu-CL reaction with cadmium telluride (CdTe) capped with thioglycolic acid has been used for the determination of methionine (with oxidant IO4) [73] and phenacetin [74] and chrysoidine (with oxidant H2O2) [75].

The enhancement property of Lu-N-bromosuccinimide with silicon hybride quantum dots (QDs) has been used for the determination of carbon QDs [76].

Table-1.1: Applications of enhanced FI-Lu-CL reaction in the presence of different oxidants.

CL-Reaction###Sample matrix###Analyte###Calibration range###Limit of detection###Sample throughput(h-1)###R2###Ref

Dissolved Oxygen###Rice and human

Lu-O2-Co(II)###serum samples###Cadmium###7A5x103 pmol/L###2 pmol/L###100###0.9989###25

Lu-O2###Human serum samples###Fentanyl citrate###1A7x102 pg/mL###3x10-1 pg/mL###120###*NA###26

###Fenvalerate, deltamethrin, isulfoton,

###isofenphos-methyl, malathion,

###0.9955-

LuAO2###Pesticides action in vivo###isocarbophos, carbaryl, dimethoate,###3x10-1A3x101 nmol/L###3x10-3A1x10-2 nmol/L###**NG###27

###0.9975

###dipterex, methomyl, acephate,

###methamidophos

Hydrogen peroxide

Lu-H2O2###Iron ores (Northamptos-shire and Sinter)###Fe (II) ion###1x10-2A2.5x101 ug/mL###3.2x101 pg/mL###NG###0.9736###28

Lu-H2O2###NG###Fe(III)###5x10-1A1x101 mg/L###2.5x10-2 mg/L###144###NG###29

Lu-H2O2###Water samples###Chromium(III)###1x10-2A1x102 mg/L###6.2 g/L###120###0.9951###30

###Fe(II) and

Lu-Fe(II)-H2O2###Organic rich seawater###NG###4x10-2 and 1x10-1 nM###160###NG###31

###H2O2

LuAH2O2ACo(II)###Human urine###Creatinine###1x10-7 A3x10-5 mol/L###7.2x10-8 mol/L###~60###0.996###32

Lu-H2O2###Bovine Serum Albumin###Bovine Serum###2.5x10-9A1x10-6 mol/L###5.8x10-10 mol/L###112###NA###33

###1.0A3x101 M

###1.0A3x101 M and###0.9773

Lu-H2O2-ATP###Biological fluids###Histidineand Lysine###and###NG###34

###1.0A6x101 M###0.9907

###1.0A6x101 M

Lu-H2O2###Pharmaceutical capsules###Tryptophan###1.0x106A1.0x103 mol/L###7.5x107mol/L###45###0.9989###35

Lu-H2O2###Animal eggs###Sarafloxacin###2.0x10-7A8.0x10-5 g/L###4.0x10-8 g/L###NG###0.9992###36

###70

###5x10-2A1.5x101 g/mL###8x10-3 g/mL

###Vitamin A###70

Lu- H2O2- Cu(II)###Pharmaceutical formulations.###1x10-1A2x101 g/mL###5x10-3 g/mL###NG###37

###Vitamin C Rose Bengal###30

###1x10-1A5x101 g/mL###5x10-2 g/mL

###Hexamethylenetriperoxidediamine,###0.98 A 0.99

###1.0A2x102 uM###5x10-1 uM

Lu- H2O2-Cu(II)###Organic peroxide explosives###triacetonetriperoxide and methyl-lethyl###NG###38

###2x10A2x102 uM###1x101 uM

###ketone peroxide###0.97

Lu-H2O2-Au###Human blood samples###glycated hemoglobin###5x10A2x102 g/mL,###3.5x102 ng/mL###NG###0.982###39

Lu-PIP-H2O2 AHRP###Prok and prok liver###Salbutamol###5x10-1A1x102 ng/mL###1.5x10-1 ng/mL###NG###0.9938###40

###Fe3O4###2.0-1x102 nM###8x10-1 nM###0.9970

###Environmental samples (unpolluted river

Lu-H2O2###AgNPs###2.5-8x101 pM###1.9 pM###NG###0.9989###41

###water to raw sewage)

###AuNPs###1.0-5x101 pM###1.1pM###0.9958

LuAH2O2###Human serum samples###Prealbumin###5x10-2A1x103 g/L###1x10-2 g/L###35###0.9659###42

Potassium Ferricyanide

Lu- K3Fe(CN)6###Injection###Mezlocillin sodium###2x10-7A5x10-5 g/mL###6.8x10-9 g/mL###NA###NA###43

Lu-K3Fe(CN)6###Synthetic and real sample###Ceftezole sodium###1x10-7A1x10-4 g/mL###3x10-8 g/mL###NA###NA###44

Iodate

Lu--IO4###Serum samples###Amikacin sulfate###4x10-9A4x10-6 g/mL###1.2x10-9 g/mL###NG###0.9978###45

###Human milk, fresh cow's milk and infant

Lu-IO4###Retinyl acetate###1.0A1x10-5 mol/L###5x10-7 mol/L###90###0.9996###46

###milk-based formulas

Potassium permanganate

Lu -KMnO4###Water Samples###Fenpyroximate###5x10-3A1x10-1 g/ml###2.5x10-1 ng/ml###NG###0.993###47

Lu-KMnO4###Water samples###Fungicide azoxystrobin###1.0A1x102ng/mL###1.3x10-1 ng/mL###NG###0.998###48

Lu-KMnO4###Pharmaceutical preparations###L-thyroxine###5x10-8A3x10-6 mol/L###8.9x10-9 mol/L###140###0.9952###49

Other oxidants

###Platinum group elements for geochemical

Lu-5-sulfosalicylic acid###analysis certified reference materials###Platinum###2x10-3A4x10-1g/mL###9x10-1 ng/mL###NG###0.9996###50

###GBW07291 and GBW07293

Lu-diperiodatocuprate(III) Urine samples.###Ractopamine###1x10-9A1x10-6 g/mL###3.4x10-10 g/mL###NG###NG###51

LuABSA###Air and beer samples###Formaldehyde###7.0 ~ 1x103 pmol/L###2.5 pmol/L###112###NG###52

Lu-hydrazine###Human blood and serum###Hemoglobin###5x10-9A6x10-5 g/mL###5.8x10-10 g/mL###53

###2,20

###-([1,10

LuAurea peroxide###Flour###-biphenyl]-4,40###1.0A6x102 nmol/L###1x10-1 nmol/L###NG###0.9978###54

###-diyldi-2,1-ethenediyl)bis-benzenesulfonic

###acid disodium salt

LuAN-bromosuccinimide###Smoked food samples###Phenols###1x10-7A1x10-3 mol/L###3x10-8 mol/L###4###0.992###55

Lu-Percarbonate and###Co(II)###2.5x10-1A2.5 ng/mL###1.510-1 ng/mL###0.9998

###Water samples###NA###56

Lu-Percarbonate###Cu(II)###2x10-1A1.4 g/mL###1.8x10-1 g/mL###0.9998

Lu-benzoyl peroxide###Flour brightener###Benzoyl peroxide###1x10-6A1x10-8 g/mL###2x10-9 g/mL###NA###NA###57

Lu-isoamyl nitrite###Pharmaceutical preparations###Isoamyl nitrite###1x10-1A1x101 mM###3x10-2 mM###30###0.997###58

Table-1.2: Applications of enhanced FI-Lu-CL reaction with nanomaterials and semiconductors.

CL-Reaction###Sample matrix###Analyte###Calibration range###Limit of detection###Sample###R2###Ref

###throughput(h-1)

LuAH2O2-Au-NPs###Mineral water samples###Manganese(II)###1.0A6x102 nM,###3x10-1 nM###**NG###0.9952###60

###Human###1x10A1 A1.0 ng/mL###0.9994

Lu-H2O2 -HRP-Au-NP###Human serum samples###3x10A2 ng/mL###NG###61

###immunoglobin G###1.0A1x101 ng/mL###0.9965

###Tap water,

###1x10-10A1x10-6 mol/L

Lu-K3Fe(CN)6-Au-NPs###Vitamine C tablet and Orange###Ascorbic acid###2x10A11 mol/L###NG###0.998###62

###juice

Lu- H2O2-Ag-NPs###Milk, foodstuffs, and honey samples###Chloramphenicol###1x10-8A1x10-6 g/mL###7.6x10-9 g/mL###NG###0.994###63

Lu-H2O2-Fe-MOFs###Human serum###Alpha-fetoprotein###5.0A1x102 pg/mL###3.0 pg/mL###NG###0.9972###64

###Water samples and hydroquinone

Lu- K3Fe(CN)6-Fe3O4-NPs###Hydroquinone###2x10-7A1x10-5 mg/mL,###7.9x10-8 mg/mL###NG###0.997###65

###cream

Lu-H2O2-ZnO-NPs###Rainwater###H2O2###6x10-2 A2x101 mol/L###1.6x10-2 mol/L###*NA###NA###66

Lu-H2O2 Auricase- Co3O4 ANPs###Human serum###Serum uric acid###6x10-1A9 M###1x10-1 M###NG###0.9985###67

###2x10-2A2x102 mg/L###1.5

Lu-H2O2AMMB-HRP-Si-NPs###Water samples###Microcystin-LR###6x10-3 mg/L###0.997###68

###1x10-8A3x10-6 mol/L

###H2O2###5x10-9 mol/L

Lu-H2O2-Co-Fe-LDH- NPs###Milk, rain water and serum sample###5x10-8A1x10-6 mol/L###80###0.9945###69

###glucose###2x10-8 mol/L

Lu-KIO4-Ag-Co###Synthesized samples.###Pyrogallic acid###1x10-10A1x10-5 g/mL###NG###NG###0.9971###70

LuAKMnO4ACuO-nanosheets###Water samples and human serum###Meropenem###5x10-3A6.0 mg/L###3.6x10-3 mg/L###120###0.9931###71

###Environmental water and

Lu-H2O2-CuO-nanosheets###Cloxacillin sodium###5x10-2A3x101 mg/L###2.6x10-2 mg/L###30###0.995###72

###pharmaceutical preparations

Lu-KIO4-CdTe-QDs###Pharmaceutical preparations###Methionine###1x10-8A1x10-5 g/mL###6.6x10-9 g/mL###NG###0.9995###73

###Qutong tablets and Children's###8.2x10-10

Lu-H2O2-CdTe QDs###Phenacetin###3x10-9A3x 10-7 mol/L###NG###0.9992###74

###keganmin powder###mol/L

Lu-H2O2-CdTe QDs###Paper and fabric cloth###Chrysoidine###1x10- 7A1x10- 5 mol/L###3.2x10- 8 mol/L###NG###0.9967###75

Lu-N-bromosuccinimide###Biomolecule conjugates###Carbon dots###1.25x10-3A2x10-2 mg/mL###6x10-4 mg/mL###NG###0.9985###76

LuminolAH2O2- PtCox/graphene###Commercial glucose sample###Glucose###3.33A2.77x101 mol/L###3.33 mol/L###NG###0.994###77

###Human serum

LuAH2O2-MMB-graphene###Thrombin###5x10A15A2.5x10-10 mol/L###1.5x10A15 mol/L,###NG###0.9970###78

###samples

Lu-H2O2-MGO-MWC-NTs###Eggs###Lysozyme###5.04x10-9 A4.27x10-7 g/mL###1.9x10-9 g/mL###NA###NA###79

Lu-O2-Fe(III)-OG

###Human urine###Dopamine###5x10-2A6x10-1 M###2.0410-2 M###NG###0.9928###80

Lu-O2-Co(II)-MOF###Pharmaceutical injections###Cysteine###2.0A1x101 M###4.9x10-1 M###NG###0.9933###81

Inhibition of FI-Lu-CL reaction in the presence of different oxidants

Inhibition of CL reactions is due to the decreasing or completely abolishing the interactions of CL reagents with other chemical species. Two types of inhibition are encountered that are, static and dynamic inhibitions. In former, interaction between the luminescent species and the inhibitor takes place in the ground state, producing a non-luminescent complex, whereas, in latter, a reaction takes place between the luminescent species and inhibitor during the lifetime of the excited state of the former [19]. Both types of inhibition have been commonly employed in analytical procedures for the quantification of analyte (Table 2.1 and 2.2). The inhibition of Lu-CL reactions with dissolved oxygen in the presence of different catalysts can be inhibited by several analytes, such as uric acid (Co(II) as a catalyst) [82], pseudoephedrine (pepsin as acatalyst) [83] and lanthanides [84] (Table 2.1).

Using H2O2, the inhibition of Lu-CL reaction has been used for the determination of ethylene glycol (oxidizing by bromine) [85], dibutyle phthalate(using myoglobin) [86], clenbuterol (immunosesor prepared coating-antigen immobilized on beads of carboxylic resin online incorporated in CL-reaction) [87], gentamicin (using cupper(II) catalyst) [88], diethylstilbestrol (using cobalt(II) catalyst) [89], omeprazole (using peroxynitrite) [90], hydroquinone (using Jacobsen's catalyst) [91], acetylsalicylic acid (using K3Fe(CN)6) [92], propyl gallate (using high-performance liquid chromatographic separation) [93] and eight catechins (using phase separation multiphase annular flow) [94]. The inhibition of Lu-CL reaction with K3Fe(CN)6) as oxidant has been used for the determination of 2-methoxyestradiol [95], estradiol valerate (with zinc deuteroporphyrin-ZnDP) [96] and ascorbic acid and rutin [97] (Table 2b).

Using oxidizing agent KMnO4, diclofenac sodium has been determined [98] and with hypochloride, 6-mercaptopurine (using silver(III) complex [99] and captopril [100] have been determined. A simple Lu-CL reaction with bovine serum albumin (BSA) has been used for the determination of roxithromycin [101], clarithromycin [102], diphacinone [103], diacerein [104] and trichlorofon (synthesizing molecularly imprinted polymer as an adsorbent) [105].The Lu-CL reaction with sulfobutylether-[beta]-cyclodextrin(SEB-[beta]-CD) has been employed for the detection of perhenazine [106] and clozapine [107]. The Lu-CL reaction with different compounds have been used for several analyte determinations, such as chloroauric acid-lysozyme for captopril [108], N-hydroxyphthalimide for super oxide dismutase, uric acid and cobalt(II) [109], N-bromosuccinimide for uric acid [110], 1,1-diphenyl-2-picrylhydrazyl for scutellarin [111] and chymotrypsin for rutin[112].

Inhibition of FI-Lu-CL reaction in the presence nanomaterials

The enhancement of classical CL reactions with NPs has already been discussed. A variety of analyte inhibit these NPs induced CL reactions, providing a source for the development of a number of sensitive procedures of analysis (Table 2.2). The Lu-H2O2-CL-reaction enhanced by zinc-oxide-NPs could be inhibited by analyte carvedilol [113]. The Lu-K3Fe(CN)6-CL-reaction enhanced by silver-NPs could be inhibited by analyte 2-methoxyestradiol [114].The copper oxide NSs enhanced Lu-H2O2-CL-reaction could be inhibited by vancomycin hydrochloride [115]. The same CL-reaction enhanced with graphene oxide (GO) and copper metal-organic framework (MOF) could be inhibited by ascorbic acid [116] and puerarin [117]. The Lu-H2O2-CL-reaction enhanced by Quantum dots (QDs) could be inhibited by hydroquinone (using CdTe-QDs) [118] and ranitidine (N,S co-doped carbon-QDs) [119].

Flow Injection-Lu-CL reaction in chemical analyses

Flow injection in conjugation with CL-detection is well suited for the assays of total antioxidant capacity (TAC) of several important samples due its sensitivity and simple instrumentation (Table 3). The antioxidant compounds attenuate the Lu-CL-reaction because of their reactive oxygen scavenging property. On the basis of their scavenging property, TAC of flavonoids [120] and polysaccharides [121] from tussilagofarfara, polyphenols in apple [122], polygonumcuspidatum (spectrum-effect integrated-HPLC separation) [123], different wines samples [124], hibiscus flowers [125], cardiovascular herbal medicines (HPLC-MS/MS assays) [126] and vitamin and pharmaceuticals [127] have been determined (Table 3). The inhibition of Lu-cyclodextrin-CL reaction has been used for the characterization of five important therapeutic phenolic acids (ferulic acid, vanillic acid, gallic acid, protocatechuic acid and caffeic acid) with sulfobutyl ether-[beta]-cyclodextrin[128].

Similarly, the interaction behavior of lysozyme with lanthanides (Ln(III)) has been studied by inhibition of Lu-lusozyme-CL reaction [129], antibiotic to bovine serum albumin with Lu-BSA-CL reaction [130] and different pesticides on enzyme catalase with Lu-CL reaction enhancement [27]. The determination of affinity of monoclonal antibody and hapten with Lu-CL reaction enhancement has been reported [131].

Table-2.1: Applications of inhibited FI-Lu-CL reaction in the presence of different oxidants.

CL-Reaction###Sample matrix###Analyte###Calibration range###Limit of detection###Sample###R2###Ref

###throughput(h-1)

Dissolved oxygen

Lu-O2-Co(II)###Human Urine and human serum###Uric acid###3.0A5x102 nmol/L###1.0 nmol/L###100###0.9982###82

Lu-O2-pepsin###Rat Serum###Pseudoephedrine###1x10-11x102 nmol/mL###3x10-2 nmol/mL###90###0.995###83

###Complexes admixtures of###84

Lu-O2###Lanthanide ion###3x10-1A5x102 nmol/L###**NG###NG###0.9952

###lanthanide

Hydrogen Peroxide

Lu-H2O2-Br###Antifreeze samples###Ethylene glycol###3.5x10A4.4x102 ug/mL###3.2x101 ug/mL###NG###0.9979###85

LuA H2O2-myoglobin###Wine###Dibutyl phthalate###1x10-1A1x102 pg/mL###3x10-2 pg/mL###120###0.9988###86

LuAH2O2 -p-iodophenolAHRP###Clenbuterol residue###Clenbuterol###4x10-1A1.2x102 ng/mL###2x10-2 ng/mL###NG###0.999###87

###Pharmaceutical###1.0A1x101 mg/L and 1x101A###0.996

Lu-AH2O2ACu(II)###Gentamicin###1x10-1 mg/L###120###88

###formulations and water samples###3x101 mg/L.###0.967

###6x10-10A1x10-8 g/mL and###-10

Lu-H2O2-Co(II)###Pharmaceuticals###Diethylstilbestrol###3.83x10-10 g/mL###NA###NA###89

###1x10-8A 1x10-7 g/mL

Lu-H2O2-NO2-###Pharmaceutical products###Omeprazole###3.0A1.5x101 ug/mL###1.3 ug/mL###NG###0.9987###90

LuAH2O2AJacobsen's catalyst###Water samples###Hydroquinone###6x10-10A1x10-8 g/mL###1x10-10 g/mL###NG###0.9947###91

###Acetylsalicylic Acid

LuAH2O2-K3Fe(CN)6###Pharmaceutical Formulations###2.5A1.25x10-2 g/mL###5x10-1 g/mL###75###0.9985###92

###(aspirin)

LuAH2O2###edible oil###Propyl gallate###9x10-6 A1x10 mol/L###2x10-4-7mol/L###NG###0.9934###93

Lu- H2O2###Commercial green teas###Catechin###5x10-2A1 mM###5x10-2 mM###-8###0.985###94

Potassium Ferricyanide

###Synthetic and mouse plasma

Lu-K3Fe(CN)6###2-methoxyestradiol###8x10-9A1x10-7 g/mL###8.4x10-10 g/mL###60###0.9992###95

###samples

Lu-K3Fe(CN)6-zinc###Pharmaceutical preparations

###Estradiol valerate###8x10-8 A1.0x10 g/mL###3.5x10-5 g/mL###NG###0.9946###96

deuteroporphyrin###and human serum

###Ascorbic acid###1x10-1A2x101 mg/L###8.9x10-3 mg/L

Lu- K3Fe(CN)6###Rutin tablets and human urine###NG###NG###97

###Rutin###2x10-2A6x10-1 mg/L###4.5x10-3 mg/L

Other oxidants

Lu- KMnO4###Pharmaceutical formulations###Diclofenac sodium###5.0A4.5x10-1 ug/mL###2.5 ug/mL###180###0.9962###98

LuA [Ag(HIO6)2]5-###Tablet,serum and urine samples 6-Mercaptopurine###2x10-9A3.0x10-8 g/mL###3.7x10-1 g/mL###NG###0.9982###99

Lu -hypochlorite###pharmaceutical formulations###Captopril###2x101A1.5x102 mol/L###2.0 mol/L###164###0.997###100

###Human saliva and serum

LuABSA###Roxithromycin###6x10-1A1x103 pmol/L###2x10-1 pmol/L###120###0.97###101

###samples

LuABSA###Human saliva and urine###Clarithromycin###7.5x10-4 A2.0 ng/mL###2.5x10-4 ng/mL###100###0.9980###102

###Human gastric juice and serum

LuABSA###Diphacinone###5.0A5x103 pg/mL###2.0 pg/mL###120###NG###103

###samples

###Pharmaceutical Formulation,

Lu- BSA###human saliva, and serum###Diacerein###5.0A7x10-3 pg/mL###1.0 pg/mL###120###0.9968###104

###samples

Lu- H2O2ABSA###Carrot and cabbage samples###Trichlorfon###NG###2.4x10 mg/L###NG###NG###105

###Human Urine,

Lu-SEB--CD###Serum Samples and###Perphenazine###3x10-2 A3x10 ng/mL###1x101 ng/mL###100###0.9907###106

###Pharmaceuticals

###Human urine and serum

Lu-SEB--CD###Clozapine###7x10-2A5x101 ng/mL###2x10-2 ng/mL###110###0.9960###107

###samples

LuAchloroauric acidAlysozyme###Human urine###Captopril###3x10-2 A5x10 ng/mL###3x10-21 ng/mL###100###0.9928###108

###Human urine and Co2+ in tap###Superoxide dismutase###1x10-2A2.5x10-1 ug/mL###3x10-3 ug###0.998

Lu-N-hydroxyphthalimide (NHPI)###NG###109

###and lake water###uric acid###5x101A8x103 pM###/mL###0.994

###Co2+###1x10-1A1x101 nM###1x101 pM###0.998

###3x10-2 nM

###-6###-3

LuA NBS (N-bromosuccinimide)###Sliva samples###Uric acid###6x10-6 A1x10-3 mol/L###2x10-6 mol/L###4###0.985###110

Lu-DPPH (1,1-

###5.0A2x103 ng/mL###5 ng/mL###0.9129

###Pharmaceutical injections

###Scutellarin###NG###111

diphenyl2picrylhydrazyl)###rat plasma

###4x101 A3.2x103 ng/mL###4x101 ng/mL###0.9808

###Human urine, tablets and###1x10-1A3x101 ng/mL.

LuAchymotrypsin###Rutin###3x10-2 ng/mL###120###0.9965###112

###human serum

Table-2.2: Applications of inhibited FI-Lu-CL reaction in the presence of nanomaterials.

CL-Reaction###Sample matrix###Analyte###Calibration range###Limit of detection###Sample throughput###R2###Ref

###(h-1)

LuAH2O2-ZnO-NPs###Pharmaceutical preparations###Carvedilol###5x10-8 A1x10-6 mol/L###3.25x10-9 mol/L###**NG###0.9894###113

###Serum and pharmaceutical

Lu- K3Fe(CN)6-Ag-NPs###2-methoxyestradiol###5x10-9A1x10-7 mol/L###5x10-10 mol/L###NG###0.9988###114

###preparations

###Environmental water samples,###5x10-1A1.8x101 and

###0.996

LuAH2O2ACuO-NSs###pharmaceutical formulation and###Vancomycin hydrochloride###1.8x10A4x101###1x10-1 mg/L###120###115

###0.994

###spiked human serum###mg/L

Lu-H2O2-GO-MOF###Commercial food and fruit juices###Aascorbic acid###1x10-3A1x101 M,

###3.5x10-4 M###NG###0.9935###116

Lu-O2-GO###Gegen and human urine samples###Puerarin###1x10-2A6.0 M###2.83x10-3 M###~90###0.9998###117

Lu- H2O2- Co(II)- QDs###Tap, lake and river water samples###Hydroquinone###5x10-1A5x101 nmol/L###1.7x10-1 nmol/L###NG###0.9995###118

LuAH2O2AN,S-CQDs###Capsule###Ranitidine###5x10-1A5x101 g/mL###1.2x10-1 g/mL###NG###0.9996###119

Table-3: Applications of FI-Lu-CL reaction in chemical analyses.

CL-Reaction###Sample matrix###Analyte###Ref

Inhibition of Lu-O2-CL-reaction###Flavonoids from Tussilagofarfara###Total antioxidant activity###121

Inhibition of Lu-O2-CL-reaction###Polysaccharide from Tussilagofarfara###Total antioxidant activity###122

Inhibition of Lu-O2/H2O2/OH-CL-reaction###Polyphenols fromapple###Total antioxidant activity###123

Inhibition of Lu-O2-CL-reaction###Polygonumcuspidatum###Total antioxidant activity###124

Inhibition of Lu-KMnO4-CL-reaction###Wine samples###Total antioxidant activity###125

Inhibition of Lu-O2-CL-reaction###Hibiscus flowers###Total antioxidant activity###126

Inhibition of Lu- KIO4-CL-reaction###Cardiovascular herbal medicines (Danshen injection)###Total antioxident activity (pharmacokinetic study)###127

Inhibition of Lu-H2O2-CL-reaction###Total antioxident activity (Hydroxyl Radical

###Vitamin and pharmaceuticals###Scavenginging)###128

Inhibition of Lu-cyclodextrin-CL-reaction###Sulfobutylether--cyclodextrin and phenolic acid###Characterization of binding interaction###129

Inhibition of Lu-lysozyme -CL-reaction###Lysozyme with trivalent lanthanide ions (LnIII)###Characterization of binding interaction###130

Inhibition of Lu-O2-BSA-CL-reaction###Antibiotic to bovine serum albumin###Characterization of binding interaction###131

Enhancement of Lu-O2-CL-reaction###Pesticides action in vivo###Characterization of binding interaction###27

Enhancement of Lu-K3[Fe(CN)6]-Terbutaline-CL-###Hapten and monoclonal antibody###Antibody affinity###132

reaction

Conclusions

The technique of flow injection is a powerful tool for the routine analysis of important analytes of interest in various samples. This technique provides the advantages of versatility, high sample throughput, requires no skilled operators, rapid mixing of sample, standards and reagents, limits the human exposure to the hazardous physical and chemical parameters, extra environmentally friendly, various working modes, online sample pre-treatment facility, consume less amounts of reagents, portable and well suited for field analyses and application of different detection systems. Chemiluminescence (in liquid-phase) is the fourth most widely employed detection system in FI techniques after UV/Visible, fluorescence and amperometry [132]. It is because; CL provides high sensitivities, selectivity due to a limited number of CL reagents available and wide dynamic range. FI- CL procedures have made the essential tool for the routine analyses in the analytical laboratories.

This review reveals that luminol is the most frequently used CL reagent in basic medium with different oxidants and nanomaterials. The use of nanomaterials has greatly improved the analytical and diagnostic characteristics of FI-CL strategies. Nanomaterials owing to their large surface area, easy synthesis and availability could help in achieving maximum sensitivities of the CL reactions i.e, a detection limit of femto molar is achieved [78]. In addition, FI-Lu-CL reactions have also been used to study the pharmacokinetics, antioxidant activity, binding interactions and anti-body affinity of different important substances. FI procedures coupled with CL detection for the determination of important analytes published in 2013 to date (up to our access) have been reviewed along with the improvements made in FI-CL procedures using metals, oxidants and nanomaterials.

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Author:Kakar, Attiq-Ur-Rehman; Khan, Naqeebullah; Samiullah; Waseem, Naeemullah Amir; Rehman, Fazal Ur
Publication:Journal of the Chemical Society of Pakistan
Article Type:Technical report
Date:Dec 31, 2018
Words:10858
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