HPLC. Spectrophotometric Measurement of Carbendazim Residue Levels in Cucumber and its Comparision with HPLC. Multivariate Curve
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1 HPLC Spectrophotometric Measurement of Carbendazim Residue Levels in Cucumber and its Comparision with HPLC ( : : ). Multivariate Curve Resolution-Alternative Least Squares(MCR-ALS). MCR-ALS.. UV-Vis. Corresponding author: v_mahdavi2@yahoo.com
2 ... :.. HPLC. HPLC. : - (MCR-ALS).(HPLC) Abstract A new, simple and accurate method is used for measuring pesticides residue. Multivariate Curve Resolution- Alternating Least Squares (MCR-ALS) has become a popular chemometric method used for the resolution of multiple component responses in unknown unresolved mixtures. The chemical discipline that uses mathematical and statistical methods to design or select optimal procedures and experiments and to provide maximum chemical information by analyzing chemical data. In this research, MCR-ALS method is proposed for spectrophotometric UV-Vis data analysis of carbendazim in aqueous solution. This method decomposes the composite signal in a data matrix into the product of concentration profiles and spectra of each pure species contributing to mixture signal. Soft modeling MCR-ALS is a much more analytical way to model experimental data using only very weak and soft assumptions. Pesticide residue of carbendazim in cucumber with different concentrations was measured. To show the ability of MCR-ALS, same samples were analyzed by HPLC. Results showed the ability of proposed method as compared with HPLC. Key words: MCR-ALS, Carbendazim, HPLC, pesticide residue.
3 :...(Vandeginste, 1987).. : :(MCR-ALS) S C C D. S.(Vives et al., 1999; Tauler & Smidle, 1994) D T * *T D = CS + E = C S + E S C D S * C *. S C S * C * S C : : -. S C T 1 * *T * *T 1 D = CTT S = C S C = CT, S = T S
4 ... :.. : -. : : -.. : -. : (MCR-ALS) - : -. EFA S=DC + - C=DS :(EFA)..
5 : (EFA)..» (SVD) «...(Maeder & Zuberbuehler, 1986) HPLC. UV MS HPLC HPLC... HPLC. UV/Vis.. HPLC
6 ... :. HPLC UV/Vis UV-Vis.. Lambda nm nm/min.. nm -. Lambda 25 CONSORT C83 ph.. ph m-file MCR-ALS. als 99 (Jaumot et al., 25) (user friendly). MATLAB 6.5. Excel. ppm.. (NaOH) (HCl) ph nm
7 :.. ph ph ph NaOH HCl NaOH HCl. ph Kg... :.... %.
8 ... :. ml C LC-1AD HPLC SCL-1A VP FCV-1AL VP. CTO-1AC VP :HPLC Shimadzu DGU-14A VP SPD-1A VP UV-Vis UV. %. nm. mm C 18 YMC. C / mm. HPLC MCR-ALS :UV-Vis.. (EFA) Evolving Factor Analysis. ph ph ph. (Panades & Ibars, 1999).
9 : Ý NH N H NHCOOCH 3 _ H + +H + N N H NHCOOCH 3 _ CH 3 COOH CH Ý 3 COOH N N H NH 2. ph. ppm -A. / / ph..... : ph< (Alford et al., 1997) ppm UV-Vis ph= /. SVD.. SVD - A C= M =ppm b= cm A=εbc - ε
10 ... :. ph=/ SVD... ph ε. ph. EFA. ( -E ). g. ph -B : ppb.. UV-Vis. ppm
11 : ssel.. ( -F ) EFA -L -I. ppb MCR-ALS. : ppb ph -C.. -G EFA.. -M -J : ppb. -H ph. ppb -K EFA. MCR-. -N ALS :HPLC ppb ppb ppb.
12 ... : 1.2 Absorbance Absorbance A Wavelength(nm) (nm) Absorbance Absorbance B Wavelength(nm) Absorbance C Wavelength(nm) Absorbance D Wavelength(nm) ph - Fig. 1- Absorptive spectra of carbendazim standard solution in ph-metric titration system A=1ppm,standard, B=1ppb,sample, C=1ppb,sample, D=1ppb,sample
13 :.8 Absorbance Wavelength(nm) - Fig. 2- Absorptive spectrum of porotonate carbendazim form 3 Molar Absorbance Absorptivity Wavelength(nm) - Fig. 3- Pure spectrum of porotonete carbendazim form Molar Absorbance Absorptivity Wavelength(nm) - Fig. 4- Pure absorptive spectrum of carbendazim without acyl
14 ... : Singular Value E Number of row row Singular Singular Value Value F F Number of row Singular Value G Number of row G Singular Value H Number of row row H EFA - : : : : ph Fig. 5- Estimated concentration profile from EFA in ph-metric titration: bold continuese line: protonic form, dotted line: neutral form, regular continues line: deacyl form E=1ppm,standard, F=1ppb,sample, G=1ppb,sample, H=1ppb,sample
15 : Concentration(mol/L) Concentration(mol/L) Concentration (mol/l) Concentration(mol/L) 1.2E-7 9.E-8 6.E-8 3.E-8.E E-7 8.E-8 4.E-8 ph J.E E-9 9.E-1 6.E-1 3.E-1 ph K : MCR-ALS - : : Fig. 6- Real concentration profile from MCR-ALS. bold continuese line: protonic form, dotted line: neutral form, regular continues line: deacyl form. I=1ppb,sample, J=1ppb,sample, K=1ppb,sample ph.e ph I I J K
16 ... : Molar Absorbance Absorptivity Molar Absorbance Absorptivity Molar Absorbance Absorptivity Wavelength(nm) Wavelength(nm) M Wavelength(nm) Wavelength (nm) N :.MCR-ALS - : : Fig. 7 -Real spectrum profile from MCR-ALS, bold continuese line: protonic form, dotted line: neutral form, regular continues line: deacyl form. L=1ppb,sample, M=1ppb,sample, N=1ppb,sample L L M N
17 : 1.2E+6 y = 1419x R 2 =.9984 Area Area 8.E+5 4.E+5.E Concentration(ppb) HPLC - Fig. 8- Calibratin curve of measured samples from HPLC method UV-Vis - Table 1- Results from UV-Vis spectrophotometry % %Recovery Calculated Concentration Real Concentration 1% ppb 13% ppb 93%.93 1 ppb HPLC - Table 2- Results from HPLC method % %Recovery Calculated Concentration Real Concentration 99% ppb 99% ppb 99%.99 1 ppb
18 ... :. ppb ppb ppb. HPLC UV-Vis. ph. HPLC. ph. HPLC HPLC.. ph MCR-ALS.. :.
19 : ALFORD, D., D. BATTY, G. BRIGGS, R. BROMILOW, D. CARTWRIGHT and et al., The Pesticide Manual, CDS Tomlin, British Crop Protection Council, UK, 182. JAUMOT, J., R. GARGALLO and R. TAULER, 25. A graphical user-friendly interface for MCR-ALS: a new tool for multivariate curve resolution in MATLAB. Chemometr. and Intell. Lab. Sys. 76: MAEDER, M. and A. D. ZUBERBUEHLER, New methods in chemistry. Anal. Chim. Acta. 181: PANADES, R. and A. IBARS, Photodecomposition of carbendazim in aqueous solutions. Water research. 34: TAULER, R. and A. K. SMIDLE, Chemometrics. Anal. Chem. Vol. 66: VANDEGINSTE, B. G. M Chemometrics, General introduction and historical development, Topics in current chemistry VIVES, M., R. GARGALLO and R. TAULER, Chemometrics. Anal. Chem. 71: Address of the author: Eng. V. MAHDAVI, Iranian Research Institute of Plant Protection, P. O. Box 1454, Tehran 19395, Iran.
20 ... :
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