Determination of Residual Acetamiprid and Imidacloprid in Unpolished Rice by Centrifugal Spin Column Clean-up and Water Mobile Phase HPLC-Diode Array

2021 ◽  
pp. 81-88
Author(s):  
Naoto Furusawa
2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.


2020 ◽  
Vol 7 (2) ◽  
pp. 101-105
Author(s):  
Nesrine T. Lamie ◽  
Hany H. Monir

Background: Cinnarizine is used to treat nausea and vomiting accompanied by motion sickness. Dimenhydrinate is used in the treatment of nausea and vomiting and dizziness. The coformulation of the two drugs showed the lowest rate of adverse effects compared to single dimenhydrinate. Objective: A fully validated ultra-performance liquid chromatographic method has been conducted for the simultaneous estimation of cinnarizine (CIN) and dimenhydrinate (DIM). Materials and Methods: The UPLC method used Acquity Column as stationary phase and mobile phase methanol: buffer (pH = 3.5 ± 0.05) and acetonitrile in the ratio of 50: 25: 25 at a flow rate of 0.2 mL/min. Detection was performed by DAD at 260 nm. Results and Discussion: Retention time was 0.71 and 1.12 min for DIM and CIN, respectively. The linearity was found to be 1-40 μg/mL and 2-80 μg/mL for CIN and DIM; respectively. Conclusion: The method was appropriately used for the quantitation of both drugs in pure form, synthetic mixtures and tablet preparation.


2006 ◽  
Vol 89 (1) ◽  
pp. 71-77 ◽  
Author(s):  
Dorota Kowalczuk ◽  
Maria Bożena Wawrzycka ◽  
Agnieszka Haratym Maj

Abstract Nifedipine (Nif) is widely used in treating cardiovascular disorders (especially hypertension) and for inhibiting preterm labor. A fully validated selective high-performance liquid chromatographic method with diode array detection, using solid-phase extraction, was developed for the determination of Nif in human serum. To assess specificity, Nif and its degradation products were separated on a Purospher RP-18 (5m, 125×4 mm) column plus a LiChrospher 100<sup/> RP-18 (5 μm, 4×4 mm) precolumn with a mobile phase of methanol10 mM aqueous trifluoroacetic acid, pH 7.3 (57 + 43, v/v); chromatographic separation was followed by UV detection at 238 nm. For toxicological analysis, Nif in the presence of other calcium-channel antagonist drugs was identified under optimum chromatographic conditions. The calibration graph was constructed over the concentration range of 12.5400 ng/mL in serum with good correlation (r 0.9956). This method was not subject to interference by other plasma components and was successfully applied to the assay of Nif in spiked human serum and in serum of women in preterm labor after sublingual administration of 30 mg Nif per day divided into 3 equal doses. The mean recovery based on the ratio of the slopes of serum and mobile phase standard curves was 96.5%. The detection and quantification limits of the drug in spiked human serum were found to be 6 and 17.5 ng/mL, respectively. Validation of the method demonstrated good intraday and interday precision, which ranged from 2.18 to 6.67% and from 6.52 to 11.93%, respectively.


2011 ◽  
Vol 94 (2) ◽  
pp. 503-512 ◽  
Author(s):  
Tarek S Belal ◽  
Rasha A Shaalan ◽  
Rim S Haggag

Abstract A simple, rapid, and selective HPLC-diode array detector method was developed for the simultaneous determination of lidocaine hydrochloride (LD) and cetylpyridinium chloride (CPC) in two combined pharmaceutical formulations. Effective chromatographic separation was achieved on a Zorbax SB-C8 (4.6 250 mm, 5 m particle size) column with gradient elution using a mobile phase composed of 0.05 M phosphoric acid and acetonitrile. The gradient elution started with 25 (v/v) acetonitrile, ramped up linearly to 85 in 5 min, and then was constant until the end of the run. The mobile phase was pumped at a flow rate of 1.2 mL/min. The multiple wavelength detector was set at 214 and 258 nm, and quantification of the analytes was based on measuring their peak areas. The retention times for LD and CPC were about 3.4 and 7.3 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to linearity, range, precision, accuracy, selectivity, robustness, LOD, and LOQ. Calibration curves were linear in the range of 5200 and 10400 g/mL for LD and CPC, respectively, with correlation coefficients >0.999. The proposed method was proven to be stability-indicating by the resolution of the two analytes from the related substance and potential impurity (2,6-dimethylaniline) as well as from forced-degradation products. The validated HPLC method was extended to the analysis of LD and CPC in two combined oral gel preparations for which the two analytes were successfully resolved from the pharmaceutical adjuvants and quantified with recoveries not less than 97.9.


2016 ◽  
Vol 11 (11) ◽  
pp. 1934578X1601101 ◽  
Author(s):  
Derya Cicek Polat ◽  
Maksut Coskun

The genus Epimedium is rich in terms of flavonoids, of which icariin, epimedin A, epimedin B and epimedin C are known especially to be biologically active. Therefore, it is important to quantify these compounds. In this study, a HPLC method coupled with DAD detection was developed and validated for the determination of icariin, epimedin A, epimedin B and epimedin C in Epimedium species growing in Turkey. The chromatographic separation was performed using a gradient system with a mobile phase of 0.1% formic acid (A) and acetonitrile (B) applied at a flow rate of 1 mL/min using a diode array detector. The highest values were, respectively, icariin 0.65%, epimedin A 0.13%, epimedin B 0.11%, epimedin C 0.06%. The highest values were obtained from the materials collected in Uzungol (Trabzon-Turkey).


2020 ◽  
Vol 12 (3) ◽  
pp. 35-45
Author(s):  
Huacheng Tang ◽  
Jiangling Qu ◽  
Dongmei Cao ◽  
Weisong Wang ◽  
Yuhao Lou

An improved quick, easy, cheap, effective, rugged, and safe (QuEChERS) method combined with high-performance liquid chromatography (HPLC) coupled to diode array detection was established for the determination of fomesafen and quizalofop-p-ethyl in beans. It is simple and efficient and can be used in most laboratories. This method optimizes four chromatographic conditions, namely, mobile phase, mobile phase ratio, flow rate, and detection wavelength. The effects of extraction agent, extraction dose, extraction time, NaCl amount, and adsorbent on the pretreatment effect were studied. The recoveries were high (92.4–117.8%), and repeatability was good (relative standard deviation [RSD] ranged from 0.35 to 4.36%). The standard solutions ranged from 0.1 to 25 ?g/mL. The detection limits of fomesafen and quizalofop-p-ethyl were 0.005 and 0.003 mg/kg, respectively.


2013 ◽  
Vol 32 (1) ◽  
pp. 299 ◽  
Author(s):  
Lenche Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska

ultraviolet–diode array detection (UV-DAD) for the simultaneous determination of atrazine, malathion, fenitrothion, and parathion residues in apple juices has been developed. For the enrichment and cleanup of compounds of interest, Supelclean ENVI-18 SPE tubes were used. Separation and quantitative determination of the analytes were performed on a LiChrospher 60 RP-select B (125 mm × 4 mm, 5 μm, Merck) analytical column, the mobile phase consisting of acetonitrile/water (55/45, V/V) in isocratic elution with the following set values: flow rate of 1 ml/min, constant column temperature at 25 oC, and UV detection at 220 nm and 270 nm. The gathered values of the investigated pesticides from the apple juice samples were in the range 94.2 %–117.2 %.  


2001 ◽  
Vol 84 (5) ◽  
pp. 1543-1550 ◽  
Author(s):  
Carlo Bicchi ◽  
Chiara Cordero ◽  
Patrizia Rubiolo ◽  
Alessandro Occelli

Abstract A method is described for the simultaneous determination of diclobutrazol, flusilazole, flutriafol, hexaconazole, paclobutrazol, and tetraconazole in apple and pear pulps used in baby food at a limit of 0.01 mg/kg. Apple and pear pulp samples are subjected to selective solid-phase microdispersion (SPMD) with SPE-ED Matrix-38 and acetone–cyclohexane, and the extracts are cleaned up on a Florisil cartridge with hexane–cyclohexane–acetone. The extracts are then analyzed by liquid chromatography with ultraviolet detection, using an octadecylsilane column with a gradient-programmed acetonitrile–water mobile phase. Recoveries were determined by spiking apple and pear pulps with the 6 pesticides under investigation at 0.1, 0.05, 0.03, and 0.01 mg/kg. Six determinations were performed at each level for each pesticide. Recoveries were ≥70% at the 0.01 mg/kg level.


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