Dry eye disease commonly known as atopic keratoconjunctivitis is an autoimmune disease of

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1 4.1. Introduction Dry eye disease commonly known as atopic keratoconjunctivitis is an autoimmune disease of eyes. The disease is characterized by lesser or some time no-significant production of tear; changes in tear composition also promote inflammation on the ocular surface are also manifested in affected eye (Bielory., 2011). For untreated patients, the risk of ocular infection increases at considerable level and clinical course of the disease may proceed up to infection, corneal ulcer and blindness (Rao., 2011; Durrani et al., 2011). CYA, which has a selective immunosuppressive effect, is used for the management of dry eye disease and several autoimmune and contingent eye diseases like posterior blepharitis, ocular rosacea, post-lasik dry eye, contact lens intolerance,, graft-versus-host disease, and herpetic stromal keratitis (Utine et al., 2010; Donnenfeld et al., 2010). CYA exerts its immunosuppressive effect by interfering with lymphocyte function through impairment of T- cell receptor transcription of the interleukin-2 gene (Oellerich et al 1995). Because of the narrow therapeutic index and significant intra- and interindividual variability in the pharmacokinetic characteristics of CYA, the therapeutic concentrations of this drug must be routinely monitored (Critical issues 1995; Schutz et al., 1998; Mahalati et al., 2000). Therapeutic drug monitoring of CYA is advocated because of its low solubility (6.6µg/ml), variable bioavailability, metabolism, and excretion among individuals (Mahalati et al., 1996; Cantarovich et al., 1999; Grevel et al., 1989). Despite routine monitoring, many patients experience adverse effects like nephrotoxicity, hepatotoxicity, neurotoxicity and gingival hyperplasia (Critical issues 1995; Schutz et al., 1998; Mahalati et al., 2000). HPLC is considered the method of choice for monitoring liver transplant recipients because of the accumulation of CYA metabolites in trough concentration blood samples (Oellerich et al., 1995). Despite these concerns, HPLC in its current form is incapable of providing routine service to a busy transplant center, and the situation is likely to become more difficult DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 54

2 because recent clinical studies have suggested that measurement of CYA concentrations at single or multiple time points in the early period (0 6 h) after CYA administration might improve clinical outcome compared with traditional trough (predose) measurements (Mahalati et al., 1999; Cantarovich et al., 1999; Grevel et al., 1989). Thus there is a growing need for a rapid, sensitive, and specific assay for CYA. The introduction of mass spectrometry (MS) coupled to liquid chromatography may solve some of these difficulties and provide an appropriate turnaround time. MS is often thought to be an expensive and difficult technique; nevertheless, it is finding increasing use in laboratories screening. In order to achieve very high level of sensitivity and fast analysis, we first time attempted the development and validation of quantification of Cyclosporine A with Ultra pressure liquid chromatography (UPLC) coupled with MS that a recent advancement in Bioanalytical instrumentation. In UPLC, smaller Bridged Ethyl Hybrid column packed with small sized (1.7 µm) particles, and ultra-high pressures are used. The small-sized particles reduce plate height and, consequently allow the number of theoretical plates to be increased (LoBrutto et al., 2008) that leads to the significant improvement in the chromatographic efficiency. Moreover, coupling of MS as detector further enhanced the detection sensitivity. First time we report here a simple but very sensitive and efficient versatile bio-analytical method for the determination of Cyclosporine A in rabbit aqueous humor, cornea, conjunctiva and blood using UPLC method with Q-TOF-MS/MS detection Material and methods Chemical and Reagents CYA as a gift sample was provided by Ranbaxy Laboratories Ltd. (Haryana, India). Chitosan (CH, deacetylation degree >80%) was received as a gift sample from India Sea Foods (India). Milli-Q water was produced in the laboratory by Milli-Q water purification system (MA, USA), whereas, HPLC grade acetonitrile was obtained from Qualigens Fine Chemicals DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 55

3 (Mumbai, India). All other chemicals and reagents used were of analytical grade and were purchased from Merck Ltd. (Mumbai, India) Ultra-Performance Liquid Chromatography (UPLC) UPLC was performed with a Waters Acquity UPLC system (Serial No# F09 UPB 920M; Model Code# UPB; Waters, MA, USA) equipped with a binary solvent delivery system, an auto-sampler, column manager and a tuneable MS detector (Serial No# JAA 272; Synapt; Waters, Manchester, UK). Chromatographic separation was performed on an Acquity UPLC BEH C18 (100mm 2.1mm, 1.7μm) column at 35±2ºC. The mobile phase consisting of Acetonitrile, Water and Formic Acid ( 0.1% v/v) in the ratio of 45:45:10 with a flow rate of 0.5 ml / min was employed for a total run time of 3 min. Data acquisition, data handling and instrument control were performed by Empower Software v Quadrapole-Time of Flight-Mass Spectrometry (Q-TOF-MS) Mass spectrometry was performed on a Waters Q-TOF Premier (Micromass MS Technologies, Manchester, UK) mass spectrometer. The nebulisation gas was set to 500 L/h, the cone gas was set to 50 L h -1 and the source temperature was set to 100ºC. The capillary voltage and sample cone voltage were set to 3.0 KV and 40 V, respectively. The Q-TOF Premier was operated in V mode with a resolution over 8500 mass with 1.0 min scan time, and 0.02 s inter-scan delay. The accurate mass and composition for the precursor ions and for the fragment ions were calculated using the MassLynx V 4.1 software incorporated in the instrument. Argon was employed as the collision gas at a pressure of 5.3 х 10-5 torr. Quantitation was performed using Synapt mass spectrometer (Q-TOF) of the transitions of m/z for with a scan time of 1.0 min, and 0.02 s inter-scan per transition. The optimum values for compound-dependent parameters like trap collision energy and transfer collision energy were set to 13.2 and 80 ev, respectively for fragmentation. DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 56

4 Sample Preparation A 50 µl aliquot of rabbit aqueous humor (blank, standard, control) was pipetted into a 1.0 ml eppendorf tube, followed by the addition of 100 µl of methanol. The samples were vortexed for 5 min followed by 5 min of centrifugation at 10,000 rpm. In similar way 50 µl of rabbit plasma was processed. The excised tissues (cornea, conjuctiva) were minced with methanol and samples were filtered through a 0.22 µm nylon filter and 10 µl of the filtrate was directly injected into the UPLC/Q-TOFMS/MS system. Prior to analysis all the samples were stored at -20 C and allowed to thaw at room temperature Calibration A stock solution of (1.0 μg/ml) was prepared by dissolving an appropriate amount of CYA in Methanol. Working standard solutions of CYA were prepared by dilution of stock solution with mobile phase. To prepare the calibration plot in plasma, aqueous humor and tissue homogenates (5% w/v homogenates of cornea and conjuctiva in deionized water), aliquots of 20μL of each sample were placed in eppendorf tubes and spiked with increasing concentrations of working standard solutions to give concentrations of 0.1, 0.5, 1, 10, 50, 100 and 200 ng/ml. Calibration standards were processed according to sample preparation procedure and were analyzed by UPLC/Q-TOF-MS/MS method Method Validation The UPLC/Q-TOF-MS/MS method was validated in terms of linearity, specificity, sensitivity, precision, accuracy, system suitability and robustness according to ICH guidelines [ICH guideline] Results and discussion Sample Preparation Sample preparation is a key procedure for the determination of analytes in biological samples. The procedure described in this paper used liquid extraction, a rather simple sample DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 57

5 preparation procedure, to eliminate the possible disturbing substances for UPLC MS/MS determination. Chromatograms obtained for mobile phase, plasma, aqueous humor, cornea and conjunctiva are shown in Fig. 4: (a), (b), (c) and (d) in the mobile phase of Acetonitrile, Water and Formic Acid (0.1% v/v) in the ratio of 45:45:10 %v/v. Other solvents studied were ethyl acetate, methanol and water, but either the recoveries were low or interferences were observed UPLC/Q-TOF-MS/MS Settings UPLC/Q-TOF-MS/MS is a powerful technique and is widely used in biological analysis. The use of quadrupole analyzer in conjugation with time-of-flight (TOF) analyzer allows accurate mass measurement with increased sensitivity. In Q-TOF, quadrupole is used to select the ion of interest and TOF measures actual mass. BEH C-18 column packed with small sized (1.7 μm) particles was selected for the chromatographic separation because it exhibited excellent peak shape and had sufficient response for. Other chromatographic condition, especially the composition of mobile phase, was optimized through several trials to obtain a good intensity of response and symmetric peaks. Formic acid, acetic acid, and ammonium acetate were tested as ionization agent candidates, and it was found that formic acid performed better than the other two in terms of intensity of the response. Finally, 0.1% formic acid in water was used as the mobile phase in positive ion mode detection. The MS full scan spectra for showed protonated precursor [M+H] + ions at (Fig. 4.1) at the optimum collision energies of 13.0 ev. Capillary voltage of 3.2 KV was used for monitoring the precursor ions (m/z ) (Fig. 4.2). Quantification was done on the basis of main product ions. DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 58

6 Figure 4.1: The MS full scan spectra for showed protonated precursor [M+H] + ions at Figure 4.2: The MS/MS scan spectra showing precursor ions (m/z ) UPLC/Q-TOF-MS/MS Validation The linearity of the detector response for CYA was evaluated by injecting a total of seven calibration (working) standard solutions (1 50 ng/ml for aqueous humor and conjunctiva, 5-50 ng/ml for plasma and 5-50 ng/ml for cornea covering the working range of the assay DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 59

7 (Fig. 4.3 to 4.7). The calibration curves were constructed by plotting peak area of CYA against corresponding concentrations. The correlation coefficient for the calibration regression line for aqueous humor, plasma, conjunctiva and cornea was found to be , , and respectively (Table 4.1). The retention time of CYA was 2.01 min and no other interfering peak was observed either by matrix or by the formulation constituents, at the retention time of the drug, demonstrating method s selectivity. LOD and LOQ were experimentally estimated by the analysis of aqueous humor, plasma, conjunctiva and cornea samples spiked with serially diluted CYA standard until the signal-to-noise ratio reached 3 and 10, respectively. LOD and LOQ were found to be 0.27 ng/ml & 1 ng/ml for Aqueous humor, 1.34ng/mL & 5.0 ng/ml for Plasma, 0.31 ng/g & 1.0 ng/g for Conjunctiva and 3.31 ng/g & 10 ng/g for Cornea respectively. Figure 4.3: UHPLC chromatograms of CYA (0.2 µg/ml). DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 60

8 Figure 4.4: UHPLC chromatograms obtained from) aqueous humor spiked with CYA (0.2 µg/ml). Figure 4.5: UHPLC chromatograms obtained from blood samples spiked with CYA (0.2 µg/ml). DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 61

9 Figure 4.6: UHPLC chromatograms obtained from conjuctiva samples spiked with CYA (0.2 µg/ml). Figure 4.7: UHPLC chromatograms obtained from cornea samples spiked with CYA (0.2 µg/ml). Precision and accuracy were determined by duplicate analysis of aqueous humor samples spiked with CYA at concentrations of 1.0 ng/ml & 25 ng/ml, plasma samples spiked with CYA at concentrations 5 ng/ml & 25 ng/ml, conjunctiva samples spiked with CYA at DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 62

10 concentrations 1 ng/g & 25 ng/g and cornea samples spiked with CYA at concentrations 10 ng/g & 30 ng/g respectively followed by their comparison with the calibration curves prepared on the same day and on three different days. Precision was expressed as the percentage coefficient of variation of measured concentrations for each calibration level, whereas accuracy was expressed as percent recovery (amount found/nominal amount 100) of drug added to the blank aqueous humor. Table 4.1 summarizes the results of intra- and interday precision and accuracy of the CYA assay. Furthermore the low value of percentage RSD (< 1.74) obtained after making small changes in the developed method indicated the robustness of the method. Table 4.1: Method validation data for Cyclosporine A in aqueous humor, plasma, Conjunctiva, Cornea Parameter Values Linearity (n=6) Range Correlation Slope± SD coefficient (r 2 ) Aqueous humor 1 50 ng/ml ± Plasma 5 50 ng/ml ±0.073 Conjunctiva 1 50 ng/g ±0.091 Cornea ng/g ±0.038 Sensitivity LOD LOQ Aqueous humor 0.27ng/mL 1.0 ng/ml Plasma 1.34 ng/ml 5.0 ng/ml Conjunctiva 0.31 ng/g 1.0 ng/g Cornea 3.31 ng/g 10 ng/g Reproducibility (n=6) CyA spiked CyA found SD Precision a Accuracy b Intraday Aqueous humor 1.0 ng/ml (LOQ) ng/ml DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 63

11 Plasma 5ng/mL ng/mL Conjunctiva 1ng/g ng/g Cornea 10ng/g ng/g Inter-day Aqueous humor 1.0 ng/ml (LOQ) ng/ml Plasma 5ng/mL ng/mL Conjunctiva 1ng/g ng/g Cornea 10ng/g ng/g a Precision as % CV (Coefficient of variation) = (Standard deviation/ Mean concentration) 100 found b Accuracy as % recovery = (Mean concentration found/concentration) 100 spiked DESIGN AND DEVELOPMENT OF NANO SIZED OCULAR DRUG DELIVERY SYSTEM 64

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