Graphitized Carbon Black Research Articles

Preparation of PEFC Electrocatalysts Using SnO2 Thin Layer Support

Pt/C is widely used as a PEFC electrocatalyst. However, Pt detachment and aggregation due to carbon support corrosion can occur. Therefore, the conventional Pt/C electrocatalyst has a difficulty in durability. We have developed Pt-based electrocatalysts dispersed on graphitized carbon black (GCB) coated with SnO2 thin layer support, achieving both high activity and high durability. Here in this study, Pt-Co alloy based electrocatalysts,Pt3Co/Sn0.98Nb0.02O2/GCB, are prepared. XRD measurement confirmed that the catalyst was supported on the oxide. STEM analysis confirmed the alloying of Pt with Co. The catalytic activity was characterized by half-cell electrochemical measurements. The electrochemical activity and pore structure were examined by preparing membrane electrode assemblies (MEA) usingPt3Co/Sn0.98Nb0.02O2/GCB as the cathode catalyst.

Introducing a low-cost jute activated carbon as a novel cleanup agent in multiclass pesticide residue analysis using gas chromatography tandem mass spectrometry

For the first time, jute activated carbon (JAC), a byproduct of the jute industry, was characterised and evaluated for its cleanup efficiency in a mixture of 181 multiclass pesticide residue testing using gas chromatography tandem mass spectrometry (GC-MS/MS). Four commercially-important food matrices including okra, spinach, pomegranate and tea were chosen. Various physico-chemical techniques were used to characterise the material. The cleanup method involved dispersive solid phase extraction (dSPE) using a combination of JAC (5 mg) with 25 mg of primary secondary amine per mL of the sample extract (in ethyl acetate). The findings demonstrated a lower matrix effect and higher signal-to-noise ratio were recorded for JAC. Overall, the method offered satisfactory recoveries for most of the pesticides in all the tested matrices. The cleanup effectiveness of JAC showed superiority over the commercially available, non-renewable dSPE sorbent viz. graphitised carbon black (GCB). With a production cost of only US Dollar ~10/kg, JAC is a low-cost alternative to commercial GCB (cost = US Dollar 11–12/g). The study valorises the potential of JAC and anticipates its large-scale application in food testing laboratories.

Disperse Solid-Phase Extraction Cleanup for the Determination of 1-Deoxynojirimycin in Mulberry Leaves with Ultraperformance Liquid Chromatography-Tandem Mass Spectrometry

A new determination method of 1-deoxynojirimycin (1-DNJ) in mulberry leaves based on ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed. Dried and crushed mulberry leaves’ sample was extracted by MeCN-water solvent, purified by graphitized carbon black (GCB) and primary secondary amine (PSA) to remove organic acids and pigments, and then analyzed after attenuation and filtration. The calibration curve showed linearity in the concentration range of 10–500 ng/mL, with the correlation coefficient of 0.998. Recoveries of spiked 1-DNJ at three fortification levels ranged from 94.6% to 96.4%, with relative standard derivation below 1.2%. Additionally, the matrix effect was assessed as negligible. Compared with methods by gas chromatography (GC) and liquid chromatography (LC) via real sample detection, the proposed method acquired better stability and detection efficiency. These results proved that this method has advantages of simple operation, complete purification, small pretreatment loss, good precision and accuracy, and high determination specificity, which is suitable for massive monitoring and precise quantitation of 1-DNJ in mulberry leaves.

Development of multi-residue extraction procedures using QuEChERS and liquid chromatography tandem mass spectrometry for the determination of different types of organic pollutants in mussel.

This study aimed to develop multi-residue methods for the extraction of organic pollutants in mussels (Mytilus galloprovincialis), including 11 pharmaceuticals, 5 pesticides, 5 perfluoroalkyl substances (PFASs) and 2 illicit drugs. The combination of 4 different QuEChERS methods and 12 clean-ups (a total of 44 combinations) was tested. QuEChERS included acidified (AQ), non-acidified (SQ) and their miniaturized versions. The clean-ups included 6 different conventional dispersive solid phase extraction (dSPE) plus 2 enhanced matrix removal (EMR-Lipid) and 4 SPE procedures (including sorbents focused on phospholipid removal and polymer-based). After sample analysis via HPLC-MS/MS, the three methods that provided the best results were validated in terms of linearity, accuracy, precision, sensitivity and matrix effect. The methods selected were the combination of (i) SQ and EMR-Lipid, (ii) AQ and Z-sep+ bulk-based dSPE and (iii) AQ and graphitized carbon black (GCB)-based dSPE. Recoveries at two concentration levels (50 and 500ng/g) ranged 54-124%, 59-124% and 60-127%, respectively, and limits of quantification (LOQs) were < 30ng/g for most analytes using any of the methods. The three methods were tested in non-spiked mussel samples purchased in local markets, but organic pollutants were not detected in any sample. However, the methods probed to successfully extract a wide range of organic pollutants families in mussel samples from the market and from bioaccumulation trials.

Design and application of special solid phase extraction column for three cannabinol compounds in hemp

大麻中的主要成分大麻二酚(CBD)、大麻酚(CBN)和Δ9-四氢大麻酚(Δ9-THC)的含量决定了其性质和应用。在液相色谱分析中,由于大麻提取液中含有较多杂质,需要净化。该文基于大麻中CBD、CBN和Δ9-THC的结构特征及样品基质组成,根据中性氧化铝、硅酸镁和石墨化炭黑的不同表面特征,考察了这3种吸附剂对大麻提取液中叶绿素、多糖、高级脂肪酸酯及重金属离子的去除率和对3种大麻酚的回收率,确定了3种吸附剂的用量分别为1.80 g、0.15 g、0.05 g混合装填成的2 g/6 mL小柱为3种大麻酚类化合物测定的专用固相萃取柱。该小柱对大麻乙酸乙酯-甲醇提取液样品中CBD、CBN和Δ9-THC的回收率分别为98.9%, 95.7%和99.2%,对叶黄素、叶绿素a和叶绿素b的去除率分别为96.3%、99.2%和95.5%,对总糖的去除率为98.5%,对脂肪酸甘油酯的去除率为96.9%,对重金属离子的平均去除率为85.4%。优化了色谱分析条件,采用Eclipse Plus C18色谱柱(50 mm×2.1 mm, 1.8 μm),在1%乙酸水溶液-乙腈(30:70, v/v)流动相条件下等度洗脱,流速为0.5 mL/min,柱温为30 ℃,检测波长为210 nm,进样量为1 μL,在10 min内可完成样品分析。方法学考察表明,在0.5~50 mg/L范围内,CBD、CBN和Δ9-THC的液相色谱峰面积与其质量浓度呈良好的线性关系,相关系数(R2)分别为0.9983、0.9995和0.9981,检出限分别为0.45 μg/L、0.53 μg/L和0.38 μg/L,加标回收率为90.3%~97.0%、93.7%~95.6%、90.8%~96.1%,相对标准偏差(RSD)分别为2.2%~6.1%、4.1%~8.0%、2.4%~4.8%。研究结果表明,该文以中性氧化铝、硅酸镁和石墨化炭黑制作的复合型大麻酚类成分测定专用固相萃取柱在大麻植物中3种酚类化合物的测定中具有净化杂质、防止色谱柱污染的功能。由于大麻不同部位的化学成分存在差异,在后续的研究中,还要进一步考察小柱对其他杂质的去除情况,使得制备的固相萃取小柱更具有普适性。

Determination of atmospheric organochlorine pesticides using isotope dilution high-resolution gas chromatography/high-resolution mass spectrometry

建立了测定大气中25种有机氯农药(OCPs)的同位素稀释-高分辨气相色谱/高分辨质谱法(ID-HRGC/HRMS)。样品用正己烷/二氯甲烷(1:1, v/v)进行加速溶剂萃取(ASE)。通过柱洗脱实验、单柱和组合柱净化实验,最终确定样品的净化方案为弗罗里硅土固相萃取柱和石墨化炭黑固相萃取柱组合净化。样品萃取液净化后进行HRGC/HRMS分析。采用平均相对响应因子(RRF)法对样品中目标物进行定量,6点校准溶液RRF的相对标准偏差(RSD)均≤20%。线性范围为0.4~800 μg/L,相关系数R2均>0.992。对空白样品依次进行100 pg、400 pg和15 ng水平下的加标试验,各添加水平下OCPs测定值的RSD为0.64%~16%,加标回收率为67.2%~135%。穿透试验表明,滤膜+聚氨酯泡沫/聚氨酯泡沫作为吸附介质的大体积主动大气采样器(AAS)在采集环境空气时,五氯苯极易发生穿透,有效采样模式待进一步研究。在上述采样模式下,六氯苯的有效采样体积较小,标准状态(101.325 kPa, 273 K)采样体积应≤30 m3,其他OCPs应≤1200 m3。以上述体积计算,25种目标化合物的检出限为0.002~0.7 pg/m3。对北京环境空气样品分析测定,结果显示除反式-环氧七氯、异狄氏剂、顺式-九氯和4,4'-滴滴滴在部分样品中未检出外,其他OCPs均为100%检出;六氯苯浓度在514~563 pg/m3之间,其他OCPs的浓度在0.01~18.9 pg/m3之间;替代标回收率为33.9%~155%。由于现有相关监测标准的仪器灵敏度较低、方法检出限较高,已无法满足目前空气中痕量OCPs的测定需求,因此亟待修订新的高灵敏度监测方法标准。该方法适用于目前大气中OCPs的超痕量水平分析,为新标准的制订奠定基础,也为国家履行相关国际公约提供有力技术指导。

Determination of quintrione in rice, rice husk and rice straw and exploration of its dissipation from rice straw

A rapid and sensitive method for the identification and quantification of quintrione residue in brown rice, rice husk, and rice straw matrices was developed and validated. Samples were extracted with acetonitrile, purified with octadecylsilane (C18) and graphitized carbon black (GCB) sorbents, and quantified using ultrahigh-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The developed method exhibited excellent linearity (R2 ≥ 0.9988), and the limit of quantitation was 2 μg/kg in all matrices. The method also had outstanding trueness and recoveries (90.5–111.1%) at four spiked levels (2, 20, 200, and 2000 μg/kg) with intraday and interday precisions of 0.7–6.5% and 5.2–11.8%, respectively, in the three matrices. The applicability of the method was tested by determining the dissipation rate of quintrione in rice straw under field conditions, and the measured data fit the Hockey stick kinetic model with R2 values of 0.9349–0.9983. The half-lives of quintrione in rice straw ranged from 2.7 to 16.5 days. The results indicate that the method is effective and reliable for the detection of quintrione residue in rice paddy fields, and the dissipation data provide guidance for the safe application of quintrione.

Simultaneous analysis and risk assessment of Quizalofop, Acifluorfen, bentazone and its metabolites residues in peanut and straw under field conditions of China

In this study, we developed and validated a simple and robust method for simultaneous determination of quizalofop-p-ethyl, acifluorfen, bentazone and its two metabolites residues in peanut and straw. All samples were extracted by 0.8% formic acetonitrile (v:v) and pure water. The peanut samples were cleaned up by florisil, while the straw samples were cleansed using florisil and graphitized carbon black (GCB) by adding a desorption procedure at 55 °C. The residues were determined by a high performance liquid chromatography electro-spray ionization tandem mass spectrometry (HPLC-MS/MS). The mean recoveries of five analytes in both matrixes ranged from 77% to 110% with relative standard deviations (RSDs) <12.6%. The limits of quantification (LOQs) were 0.01 mg/kg in peanut and 0.02 mg/kg in straw. And the limits of detection (LODs) ranged from 0.047 to 0.356 μg/L. The established method was successfully applied to determine the terminal residues of the five analytes in peanut and straw samples from supervised field trials. The results showed that the residues of all analytes were less than LOQs in peanut while that was up to 0.031 mg/kg in straw. Based on residues data in peanut, chronic dietary intake risk of three pesticides was evaluated, and the results showed that the risk of all pesticides were negligible for Chinese residents.

Determination of Three Typical Metabolites of Pyrethroid Pesticides in Tea Using a Modified QuEChERS Sample Preparation by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry.

Pyrethroid pesticides are widely used on tea plants, and their residues of high frequency and concentration have received great attention. Until recently, the residues of typical metabolites of pyrethroid pesticides in tea were unknown. Herein, a modified “quick, easy, cheap, effective, rugged and safe” (QuEChERS) method for the determination of three typical metabolites of pyrethroid pesticides in tea, using ultra performance liquid chromatography tandem mass spectrometry, was developed. The mixture of florisil, octadecylsilane, and graphite carbon black was employed as modified QuEChERS adsorbents. A Kinetex C18 column achieved good separation and chromatographic peaks of all analytes. The calibration curves of 3-phenoxybenzoic acid (3-PBA) and 4-fluoro-3-phenoxybenzoic acid (4-F-3-PBA) were linear in the range of 0.1–50 ng mL−1 (determination coefficient R2 higher than 0.999), and that of cis-3-(2-chloro-3,3,3-trifluoroprop-1-en-1-yl)-2,2-dimethylcyclopropanecarboxylic acid (TFA) was in the range of 1–100 ng mL−1 (R2 higher than 0.998). The method was validated and recoveries ranged from 83.0% to 117.3%. Intra- and inter-day precisions were lower than or equal to 13.2%. The limits of quantification of 3-PBA, 4-F-3-PBA, and TFA were 5, 2, and 10 μg kg−1, respectively. A total of 22 tea samples were monitored using this method, and 3-PBA and TFA were found in two green tea samples.

Simultaneous determination of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi using ultra-performance liquid chromatography/tandem mass spectrometry

A fast, sensitive, and reliable analytical method was developed and validated for simultaneous identification and quantification of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi by ultra-performance liquid chromatography/tandem mass spectrometry (UHPLC–MS/MS). First, sample extraction was done with acetonitrile containing 1% formic acid followed by phase separation with the addition of MgSO4:NaOAc. Then, the supernatant was purified by primary secondary amine (PSA), octadecylsilane (C18), and graphitized carbon black (GCB). The linearities of the calibrations for all analytes were excellent (R2 ≥ 0.9953). Acceptable recoveries (74.5–106.4%) for all analytes were obtained with good intra- and inter- relative standard deviations of less than 14.5%. The limit of quantification (LOQs) for all analytes was 10 μg kg−1. For accurate quantification, matrix-matched calibration curve was applied to normalize the matrix effect. The results indicated that the method was suitable for detecting the three acaricides and their relevant metabolites in edible fungi.

Optimization of the Pre-treatment Method for the Determination of 9 Organophosphorus Pesticide Residues in Cabbage by Gas Chromatography

The purpose of this study was to optimize the pre-treatment process for the detection of 9 organophosphorus pesticide residues in cabbage by gas chromatography, and to conduct a comparative experiment between this method and the standard method NY/T 761-2008 of the Ministry of Agriculture. The results show that the optimized pre-treatment method is to use 10 mL acetonitrile as the extractant, 150 mg N-propyl ethylenediamine (PSA) and 15 mg graphitized carbon black (GCB) as the purification agent, which can reduce the use of extractant and inorganic salt in the pre-treatment process, increase the recovery and detection limit, reduce the matrix effect and cost of instrument maintenance.

Multivariate optimization of low-temperature cleanup followed by dispersive solid-phase extraction for detection of Bisphenol A and benzophenones in infant formula

A simple and effective analytical method to determine six contaminants, including five benzophenones (BP, BP-1, BP-3, BP-8, and BP-12) and bisphenol A (BPA) in infant formulas was developed in this study. For this, a sequential experimental design was used to optimize the extraction and cleanup method using low temperature partition (LTP) combined with dispersive solid phase extraction (dSPE). The effect of primary secondary amine (PSA), sodium chloride (NaCl), graphitized carbon black (GCB), octadecyl (C18), strong anion exchanger (SAX), water, acetonitrile (ACN) and, ultrasound (US) time were evaluated using a sequential design of experiments including a Plackett-Burman, a central composite rotatable design, and the Derringer and Suich's tool. The method was validated, and it showed a limit of quantification varying from 0.06 to 2 mg.kg-1, good precision (< 20% RSD), and recovery (52-106%). The method proposed was applied to twenty-five samples of commercial infant formulas.

Equilibrium, Kinetic and Thermodynamic Studies for the Adsorption of Gemfibrozil onto Graphitized Carbon Black (GCB)

Adsorption of gemfibrozil (GF) from aqueous solution by highly/lowly graphitized carbon black (GCB-H/GCB-L) was investigated by batch and fixed-bed experiments. Results showed that the adsorption of GF onto GCB greatly depended on solution pH and graphitization of carbon. The pseudo-second-order kinetic model was found to be more appropriate in describing the adsorption processes of two GCBs. The adsorption equilibriums were well fitted with the Langmuir isotherm model, and GCB-H exhibited a higher adsorption capacity of 47.68 mg g−1 at 298 K, compared with GCB-L of 4.33 mg g−1. GCB-H achieved 69.76% GF removals in simulated water after 6 h, indicating its potential practicability. The GCBs were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FTIR), and the results indicated that the [Formula: see text]-[Formula: see text] interaction was strongly involved in the adsorption. Thermodynamic studies further suggested that the adsorption of GF on GCB-H was exothermic, which could happen spontaneously at any temperature mainly through [Formula: see text]-[Formula: see text] interaction for physical adsorption on the surface of the plane.

Development of a fast multi-residue method for the determination of succinate dehydrogenase inhibitor fungicides in cereals, vegetables and fruits by modified QuEChERS and UHPLC-MS/MS

In this study, a simple, sensitive and efficient analytical method was developed and validated for the determination of 11 fungicides in grape, potato, rice, corn, wheat and soybean using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS). The fungicides were extracted using acetonitrile, and then the extracts were cleaned up using primary secondary amine (PSA), octadecylsilane (C18) and graphitized carbon black (GCB). Method validation displayed acceptable linearities for all pesticides (R2 greater than 0.99). The calculated limits of detection and quantification were 1 μg kg−1 and 10 μg kg−1 in different matrices, respectively. It was necessary to employ matrix-matched standards for correct quantification of these fungicides in all matrices. Acceptable recoveries (75.7–104.2%) were obtained for all the target compounds with good intra-day and inter-day precisions (RSD ≤ 11.9%). The results indicated that the method is reliable for detecting these fungicides in various foods.

Adsorption of Sodium Hexadecyl Sulfate and Triton X from Binary Aqueous Solutions at Thermally Graphitized Carbon Black

Adsorption of anionic sodium hexadecyl sulfate (SHS) and nonionic Triton X surfactants with different ethoxylation degree: TX-45, TX-100 and TX-300 from their individual and mixed aqueous solutions at the surface of thermally graphitized carbon black (CB) was studied. It was found that at low solution concentrations addition of the nonionic surfactant increases the amount of SHS adsorbed from SHS/Triton X mixtures compared to SHS amount adsorbed from its individual solution. These findings might be explained by decreasing in electrostatic repulsion between SHS ions due to inclusion of the molecules of the nonionic surfactant in the mixed adsorption layer. At higher solution concentrations, adsorption of SHS decrease as a result of displacement of SHS ions from the mixed adsorption layer by Triton X molecules. It was established that the composition of the mixed adsorption layer at CB surface notably differ from the composition of the surfactant mixture in the bulk solution. The mixed adsorption layer is enriched with the molecules of the nonionic surfactants and this conclusion is confirmed by the results of measuring zeta potential of CB particles with the adsorbed surfactants.

Simultaneous determination of sibutramine and its derivatives in weight loss dietary supplements by LC-MS/MS

The liquid chromatography tandem mass spectrometry method (LC-MS/MS) was used to determine the content of sibutramine (SB), N-desmethyl sibutramine (DSB) and N-didesmethyl sibutramine (DDSB) illegaly mixed in weight loss dietary supplements. Sibutramine and its derivatives were extracted by methanol; impurities in the extract were removed by graphitized carbon black (GCB) adsorbent. The chromatographic separation of analytes took place on C18 column (100 mm x 2.1 mm, 3.5 &amp;micro;m) with a gradient mobile phase of acetonitrile and 2 mM ammonium acetate in 0.1% formic acid solution. Multiple reaction monitoring (MRM) in the positive mode was used to detect and quantify SB, DSB and DDSB at m/z 279.9/124.8; 266.0/124.8 and 252.1/125.0, respectively. The method was validated following the AOAC requirements for specificity, repeatability and recovery. Calibration curves lineared from 0.002 to 0.1 &amp;micro;g/mL for SB, DSB and DDSB. The method was successfully applied to determine the content of SB, DSB and DDSB in weight loss dietary supplements that were randomly collected from phamacies in Hanoi of three formulations of hard capsule, soft capsule and teabag. The results shown that six samples had SB and DSB with the content in the range of 0.817 - 31.7 mg/g.

Simultaneous determination of 64 pesticide residues in shellfish by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry

A method was established for the determination of 64 pesticide residues in shellfish using accelerated solvent simultaneous extraction and purification coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). The target compounds were extracted from shellfish using 90% (v/v) acetonitrile aqueous solution with 60% of the pool volume at 85℃ via a single cycle of accelerated solvent extraction. The extracts were synchronously purified with primary secondary amine (PSA) and graphitized carbon black (GCB) added to the extracting cell. After concentration, the target compounds were detected by GC-MS/MS in the multiple reaction monitoring (MRM) mode, and quantified by using the external standard method. Under the optimized conditions, good linearities were obtained for the 64 pesticides in the range of 10.0-1000 μg/L, with coefficients of determination greater than 0.989. The limits of quantification for the method were between 2.0 μg/kg and 10.0 μg/kg. At four spiked levels (5.0, 10.0, 100 μg/kg, and the LOQ level) in clam, the recoveries of all the pesticides were between 69.4% and 129.7%, with the relative standard deviations varying from 0.7% to 16.0% (n=6). The method is simple, repeatable and sensitive, and it is suitable for the screening of various pesticide residues in shellfish products.

Adsorption and Chromatographic Characteristics of Graphitized Carbon Black, Modified by Adenine with Respect to a Series of Organic Compounds

Graphitized carbon black, modified by 0.95% adenine, is selected as the main object of study. The thermodynamic characteristics of adsorption of a series of organic compounds on modified carbon black is investigated by inverse gas chromatography. Analysis of the resulting data shows that the additivity of molar changes in the internal energy of adsorption is violated in the considered sample, in a homologous series of n-alkanes and other compounds. In contrast to a series of adsorbents studied earlier, there is no violation of additivity for pairs, but there is for at least three members of the homologous series, testifying to the presence of cavities or voids with different sizes in the supramolecular structure of adenine. The sizes of the molecules for which the violation of additivity is observed allow us to estimate the sizes of the cavities in the supramolecular structure of adenine as 5.5–6 to 9–9.5 A. It was also found that modification by adenine increases the polarity of the surface. The use of adenine at Viedma ripening conditions provides the modified adsorbent the chiral recognition capability.

Development of a fast method for the determination of pesticide multiresidues in tomatoes using QuEChERS and GC–MS/MS

Here we describe the improvement of pesticide residue extraction from tomatoes by an improved QuEChERS method. Through Plackett–Burman design, 4 significant variables out of 11 potential variables were identified that could influence the relative deviation of measurements. The 11 variables were: amount of sample, C18, Na2SO4, NaCl, MgSO4, NaAc, GCB (graphitized carbon black), and PSA (primary–secondary amine); ACN volume; percentage of FA (formic acid); and centrifugation time. The amounts of GCB, Na2SO4, PSA and sample were significant variables, which were further optimized using a Box–Behnken design to predict the optimum extraction conditions. The method presented recoveries between 72.5 and 119.7%, with relative standard deviations ranging from 1.17 to 14.62% for all real samples spiked with pesticides at three different fortification levels. Overall, methods met the requirements of national standard for pesticide residue analysis. The results indicate that the improved QuEChERS method is suitable for the routine monitoring of 20 pesticides which often are detected in tomato samples.

Validation and application of a QuEChERS-based method for estimation of the half-lives of cyromazine and acetamiprid in cowpeas and soil by LC-ESI-MS/MS

ABSTRACT A rapid and sensitive method for the simultaneous determination of cyromazine and acetamiprid in cowpeas by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed. The cleanup performance by primary secondary amine (PSA), C18 and graphitised carbon black (GCB) was carried out to optimise the sample preparation step. The analytical method showed satisfactory specificity, selectivity, linearity (R2 > 0.99) and recoveries (85.8–109.0%), relative standard deviation (intra-day RSD) between 2.7% and 14%, precision (92.0–104.2%), the inter-day precision RSD between 0.49% and 9.6%. The limits of detection (LODs) for cyromazine and acetamiprid were 0.0009 mg/kg and 0.0001 mg/kg, respectively, in soil and cowpeas, and the limits of quantification (LOQs) for each was 0.001 mg/kg. The retention times of cyromazine and acetamiprid were 1.54 min and 2.37 min, respectively. The half-lives of cyromazine in cowpeas and soil were 3.13 − 11.18 d, and the half-lives of acetamiprid were 2.1–11.95 d, which indicates that they are low-persistence insecticides with the possibility of evaporating into the air. The matrix effect was compensated for by using the standard addition method. This LC-ESI (+)-MS/MS method with short run time, high sensitivity, and low matrix effects may help laboratories handle routine pesticide residue analysis in different food samples.