Determination of malathion and its residues by normal-phase high-performance liquid chromatography method

Abstract

The quality of pesticide formulations has an impact on the crop safety, environment and human health. Therefore, the development of new analytical methods for the determination of active substances in pesticide formulations in order to control their quality, as well as, their residues in food samples in order to ensure food safety, is always welcome. A new, simple, precise and accurate normal-phase high-performance liquid chromatography (NP-HPLC) method for determination of an active ingredient malathion in the commercial emulsifiable concentrate pesticide product has been developed and validated. The analysis was carried out on a LiChrosorb CN (250 x 4 mm, 5 μm) analytical column using isocratic elution with mobile phase consisted of n-hexane and dichloromethane (80/20, v/v), flow rate of 1 mL/min, constant column temperature at 25 °C and ultraviolet diode-array detection at 220 nm. The obtained values for multiple correlation coefficients (R2 ≥ 0.9990), relative standard deviation of retention times, peak areas and heights (RSD ≤ 1.14%), recoveries ranged from 98.97 to 101.62%, revealed that the developed method has a satisfactory linearity, precision and accuracy. Also, the developed method was successfully applied for determination of malathion residues in apple juice samples, after preliminary sample preparation using solid-phase extraction. Specificity, selectivity, linearity, matrix effect, precision and accuracy were tested in order to validation of this method. The obtained results were in acceptable ranges and indicated that the developed method is suitable for routine determination of malathion in the pesticide formulation, as well as for determination of malathion residues in apple juice samples. The run time of HPLC analysis was about 6 min.

Ameliorating SERS Sensitivity for Pesticide Malathion Detection with Synergistic Boosting Effect by Hydrogen Cations and Chloride Anions

“…The column temperature was 25 °C. When the injection volume was 10 μL, the retention time of malathion was about 6 min …”

“…When the injection volume was 10 μL, the retention time of malathion was about 6 min. 32 ■ RESULTS AND DISCUSSION Optimization of Halides. Halogen ions have long been used to promote the adsorption of analytes on the SERS substrate and enhance the SERS signal.…”

An Electrochemical Strategy for Detection of Trace‐Level Binapacryl Using Square‐Wave Cathodic Stripping Voltammetry

“…There are number of works on the electrochemical determination of pesticides in environmental samples [11][12][13][14][15] and commercial formulations, [16][17][18][19][20] but chromatographic methods are the most common and frequently used for the detection of pesticide residues. [21][22][23][24] In recent years, electrochemical sensors have been widely used in pesticide analysis [25][26] because fast, selective and sensitive nanosensors are constantly being developed. [27][28] On the other hand, electrochemical or voltammetric methods have many advantages in the field of practical trace analysis compared to optical or chromatographic methods such as simplicity, cheapness, precision and speed, and are suitable for on-site monitoring of environmental pollutants.…”

“…There are number of works on the electrochemical determination of pesticides in environmental samples [11–15] and commercial formulations, [16–20] but chromatographic methods are the most common and frequently used for the detection of pesticide residues [21–24] . In recent years, electrochemical sensors have been widely used in pesticide analysis [25–26] because fast, selective and sensitive nanosensors are constantly being developed [27–28] .…”

Dual-template imprinted polymer electrochemical sensor for simultaneous determination of malathion and carbendazim using graphene quantum dots

“…Reported methods for the simultaneous determination of MAL and CBZ are insufficient in the literature, [13][14][15] and there is no report on the simultaneous electrochemical detection of these pesticides. However, there are several analytical methods for the determination of MAL or CBZ, such as gas chromatography-mass spectrometry (GC-MS), 16,17 high-performance liquid chromatography (HPLC), 18,19 chemical luminescence (CL), 20,21 and capillary electrophoresis (CE). 22,23 These techniques are costly and require highly skilled personnel.…”