[Rapid determination of 15 N-nitrosamines in air-dried yak meat using one-step QuEChERS-gas chromatography-triple quadrupole mass spectrometry].

A method based on gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) coupled with one-step QuEChERS technique was developed for the simultaneous determination of 15 N-nitrosamines in air-dried yak meat. The hydration volume, extraction solvent, extracting salt, and cleaning material were optimized according to the characteristics of the N-nitrosamines and sample matrix. The optimized conditions were as follows: 10 mL of purified water for sample hydration, acetonitrile as the extraction solvent for the sample after hydration, 4.0 g of anhydrous MgSO4 and 1.0 g of NaCl as extracting salts, 500 mg of MgSO4+25 mg of C18+50 mg of PSA as cleaning materials. Favorable recoveries of the 15 N-nitrosamines were obtained when the extraction solution was incompletely dried. Thus, the final extract was dried to below 0.5 mL under a mild nitrogen stream and then redissolved to 0.5 mL with acetonitrile. After filtration, 200 µL of the sample was transferred to an autosampler vial for GC-MS/MS analysis. The 15 N-nitrosamines were determined using GC-MS/MS on a DB-HeavyWAX column (30 m×0.25 mm×0.25 µm) with an electron impact ion source in multiple-reaction monitoring (MRM) mode, and quantified using an external standard method. Under the optimized experimental conditions, the results showed that the calibration curves exhibited good linearities for the 15 N-nitrosamines, with correlation coefficients (r2) greater than 0.9990. The limits of detection (LODs) and the limits of quantification (LOQs) ranged from 0.05 to 0.20 µg/kg and from 0.10 to 0.50 µg/kg, respectively. At spiked levels of 1LOQ, 2LOQ, and 10LOQ, the average recoveries were 79.4%-102.1%, 80.6%-109.5%, and 83.0%-110.6%, respectively, and the relative standard deviations were in the range of 0.8%-16.0%. The low matrix effects of the 15 N-nitrosamines indicated the high sensitivity of the proposed method. The method was applied to detect representative commercial air-dried yak meat samples obtained using different processing techniques. Seven N-nitrosamines, including N-nitrosodimethylamine, N-nitrosodiisobutylamine, N-nitrosodibutylamine, N-methyl-N-phenylnitrous amide, N-ethyl-N-nitrosoaniline, N-nitrosopyrrolidine, and N-nitrosodiphenylamine were detected in all samples. The average contents of the seven N-nitrosamines was 0.08-20.18 µg/kg. The detection rates and average contents of the N-nitrosamines in cooked air-dried yak meat samples were higher than those in traditional raw air-dried yak meat samples. Compared with the manual QuEChERS method, the one-step QuEChERS method developed integrated the extraction and clean-up procedures into one single run, and the detection efficiency was considerably improved. The developed method is simple, rapid, highly sensitive, and insusceptible to human errors. Thus, it is useful for the determination of N-nitrosamines in air-dried yak meat and can be extended to the qualitative and quantitative analysis of N-nitrosamines in other meat products. It also provides method support and a data reference for the general determination of N-nitrosamines, which is of great significance for food safety.

Screening of 439 Pesticide Residues in Fruits and Vegetables by Gas Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and Q-TOF Spectrum Library.

Because of its unique characteristics of accurate mass full-spectrum acquisition, high resolution, and fast acquisition rates, GC-quadrupole-time-of-flight MS (GC-Q-TOF/MS) has become a powerful tool for pesticide residue analysis. In this study, a TOF accurate mass database and Q-TOF spectrum library of 439 pesticides were established, and the parameters of the TOF database were optimized. Through solid-phase extraction (SPE), whereby pesticides are extracted from fruit and vegetable substrates by using 40 mL 1% acetic acid in acetonitrile (v/v), purified by the Carbon/NH2 SPE cartridge, and finally detected by GC-Q-TOF/MS, the rapid analysis of 439 pesticides in fruits and vegetables can be achieved. The methodology verification results show that more than 70 and 91% of pesticides, spiked in fruits and vegetables with concentrations of 10 and 100 µg/kg, respectively, saw recoveries that conform to the European Commission's criterion of between 70 and 120% with RSD ≤20%. Eighty-one percent of pesticides have screening detection limits lower than 10 µg/kg, which makes this a reliable analysis technology for the monitoring of pesticide residues in fruits and vegetables. This technology was further validated for its characteristics of high precision, high speed, and high throughput through successful detection of 9817 samples during 2013-2015.

Screening of 485 Pesticide Residues in Fruits and Vegetables by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and QTOF Spectrum Library.

This paper uses the LC-quadrupole-time-of-flight MS technique to evaluate the behavioral characteristics of MS of 485 pesticides under different conditions and has developed an accurate mass database and spectra library. A high-throughput screening and confirmation method has been developed for the 485 pesticides in fruits and vegetables. Through the optimization of parameters such as accurate mass number, time of retention window, ionization forms, etc., the method has improved the accuracy of pesticide screening, thus avoiding the occurrence of false-positive and false-negative results. The method features a full scan of fragments, with 80% of pesticide qualitative points over 10, which helps increase pesticide qualitative accuracy. The abundant differences of fragment categories help realize the effective separation and qualitative identification of isomer pesticides. Four different fruits and vegetables-apples, grapes, celery, and tomatoes-were chosen to evaluate the efficiency of the method at three fortification levels of 5, 10, and 20 µg/kg, and satisfactory results were obtained. With this method, a national survey of pesticide residues was conducted between 2012 and 2015 for 12 551 samples of 146 different fruits and vegetables collected from 638 sampling points in 284 counties across 31 provincial capitals/cities directly under the central government, which provided scientific data backup for ensuring pesticide residue safety of the fruits and vegetables consumed daily by the public. Meanwhile, the big data statistical analysis of the new technique also further proves it to be of high speed, high throughput, high accuracy, high reliability, and high informatization.

High-Throughput Analytical Techniques for the Determination of the Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VII: A GC-MS, GC-MS/MS, and LC-MS/MS Study of the Degradation Profiles of Pesticide Residues in Green Tea.

GC-MS, GC-tandem MS (MS/MS), and LC-MS/MS were used to mathematically define the degradation profiles of pesticide residues in two field trials. Nineteen pesticides were studied in the first field trial and 11 in the second. The results of the field trials demonstrated that the degradation profiles of pesticide residues in green tea can be described with power functions to successfully estimate the amount of time, following pesticide application, pesticide residues appearing in tea in concentrations at and/or above the maximum residue limit (MRL) decrease to concentrations below the MRL. Stability tests on green tea samples stored at room temperature were conducted to determine whether pesticide-incurred green tea samples prepared according to the method used in the field trials would be suitable for the preparation of reference standards for laboratory-proficiency testing trials. This paper reports the results of a GC-MS, GC-MS/MS, and LC-MS/MS study, as well as the suitability of the samples prepared under these conditions for use as pesticide reference standards in tea analysis.

High-Throughput Analytical Techniques for Determination of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VI: Study of the Degradation of 271 Pesticide Residues in Aged Oolong Tea by Gas Chromatography-Tandem Mass Spectrometry and Its Application in Predicting the Residue Concentrations of Target Pesticides.

The degradation rate of 271 pesticide residues in aged Oolong tea at two spray concentrations, named a and b (a < b), were monitored for 120 days using GC-tandem MS (GC-MS/MS). To research the degradation trends and establish regression equations, determination days were plotted as horizontal ordinates and the residue concentrations of pesticide were plotted as vertical ordinates. Here, we consider the degradation equations of 271 pesticides over 40 and 120 days, summarize the degradation rates in six aspects (A-F), and discuss the degradation trends of the 271 pesticides in aged Oolong tea in detail. The results indicate that >70% of the determined pesticides coincide with the degradation regularity of trends A, B, and E, i.e., the concentration of pesticide will decrease within 4 months. Next, 20 representative pesticides were selected for further study at higher spray concentrations, named c and d (d > c > b > a), in aged Oolong tea over another 90 days. The determination days were plotted on the x-axis, and the differences between each determined result and first-time-determined value of target pesticides were plotted on the y-axis. The logarithmic function was obtained by fitting the 90-day determination results, allowing the degradation value of a target pesticide on a specific day to be calculated. These logarithmic functions at d concentration were applied to predict the residue concentrations of pesticides at c concentration. Results revealed that 70% of the 20 pesticides had the lower deviation ratios of predicted and measured results.

High Throughput Analytical Techniques for the Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea by GC/MS, GC/MS/MS, and LC/MS/MS: Collaborative Study, First Action 2014.09.

Thirty laboratories from fom North and South America, Europe, and Asia participated in this AOAC collaborative study (15 from China; five from Germany; two each from Italy and the United States; and one each from the Republic of Korea, Canada, Spain, Japan, Belgium, and India). Participants represented government regulatory, commercial testing, university, research institute, and private laboratories. The single-laboratory validated (SLV) tea method was evaluated in the collaborative study to determine the recovery and reproducibility of the method under multilaboratory conditions. Since there were no restrictions regarding the type of analytical instrumentation to use for the analyses, laboratories used a combination of equipment that included GC/MS, GC/MS/MS, and LC/MS/MS instruments from 22 different manufacturers, 21 brands of GC and LC columns, 13 different GC temperature programming profiles, 11 LC gradient elution programs, and six different vendor manufactured SPE cartridges. Even though all the analytical performance parameters for all the 653 compounds had been determined in the SLV study, guidance was obtained from an expert review panel of the AOAC Method-Centric Committee on Pesticide Residues to conduct the multilaboratory collaborative study based on 20 selected compounds that can be analyzed by GC/MS and 20 compounds that can be analyzed by LC/MS/MS. Altogether, 560 samples covering the 40 selected pesticides were analyzed in the study. These samples included green tea and oolong tea samples fortified typically at the European Union maximum residue limit for regulatory guidance and compliance, aged tea samples incurred with 20 pesticides, and green tea and oolong tea samples incurred with five pesticides. The analysis of the 560 samples generated a total of 82 459 test results by the 30 participating laboratories. One laboratory failed to meet the proficiency requirements in the precollaborative study. Therefore, its data submitted for the collaborative study were excluded from further analysis and interpretation. The results presented are therefore the 6638 analytical results obtained from the 29 remaining laboratories, which included 1977 results generated by GC/MS, 1704 results by GC/MS/MS, and 2957 results by LC/MS/MS. It was determined after application of the Grubbs and Dixon tests for outliers to the data sets that there were 65 outlier results from the 1977 GC/MS results (3.3%), 65 outlier results from the 1704 GC/MS/MS results (3.8%), and 57 outlier results out of 2957 LC/MS/MS results (1.9%), representing 0.98, 0.98, and 0.86%, respectively, of the 6638 results generated in the study. Analysis with the AOAC statistical software package also confirmed that the method is rugged, and average recovery, average concentration, RSDr, RSDR, and HorRat values all meet recovery and reproducibility criteria for use in multiple laboratories. The Study Director is recommending this method for adoption as an AOAC First Action Official MethodSM.

[Application of ICP-MS method in the determination of mineral elements in vitex honey for the classification of their geographical origins with chemometric approach].

In the present work, the contents of 38 elements of 65 vitex (Vitex negundo var. heterophylla Rehd. ) honey samples from Shunyi of Beijing, Fuping and Pingshan of Hebei province were determined by inductively coupled plasma mass spectrometry (ICP-MS). Among them, B, Na, Mg, P, K, Ca, Fe and Zn were the most abundant elements with mean contents more than 1 mg kg-1. It can be found that there were relationships between the contents of elements and the geographical origin of vitex honey samples. Taking the contents of 29 out of 38 mineral elements (Na, Mg, Al, K, Ti, V, Mn, Fe, Ni, Cu, Zn, Ga, As, Sr, Y, Mo, Cd, Ba, La, Ce, Pr, Nd, Sm, Gd, Dy, Ho, T1, Pb and U) as variables, the chemometric methods, such as principal component analysis (PCA) and back-propagation artificial neural network (BP-ANN), were applied to classify vitex honey samples according to their geographical origins. PCA reduced all of the variables to four principal components and could explain 81. 6% of the total variances. The results indicated that PCA could mainly classify the vitex honey samples into three groups. BP-ANN was explored to construct classification model of vitex honeys according to their geographical origin. For the whole data set, the overall correct classification rate and cross-validation (leave one out method) rate of proposed BP-ANN model was 100% and 95. 4%, respectively. To further test the stability of the model developed for prediction, 75% of honey samples of each geographical origin were randomly selected for the model training set, and the remaining samples were classified with the use of the constructed model. Both the overall correct classification rate and prediction rate of proposed BP-ANN model were 100%. It is concluded that the profiles of multi-element by ICP-MS with chemometric methods could be a potential and powerful tool for the classification of vitex honey samples from different geographical origins.

High-Throughput Analytical Techniques for Multiresidue, Multiclass Determination of 653 Pesticides and Chemical Pollutants in Tea-Part IV: Evaluation of the Ruggedness of the Method, Error Analysis, and Key Control Points of the Method.

A 3 month study was conducted on the ruggedness of a multiresidue method for accuracy and stability. The results indicate that in terms of Youden pair ratios of 201 pesticide aged tea samples falling approximately within 1.00-1.20 of the ratio of theoretical spraying concentrations, the differences do not exceed 5% for percentages made up by ratios of the fixed values obtained by two kinds of instruments for two teas and those made up by 18 circular determinations. However, regarding two kinds of SPE cartridges, the Cleanert TPT cartridge is higher than the ENVI-CARB+primary secondary amine (PSA) cartridge by 10%. Pertaining to RSD values of "parallel samples" and whether it is green tea or Woolong tea, the percentages of RSD≤15% values of the parallel samples all exceed 88%. Whether it is the first or circular determination for two teas and analytical results from two kinds of instruments, the percentages of RSD≤15% values have a difference of less than 6%, while the TPT cartridge is better than ENVI-CARB+PSA by above 6% for the two cartridges. Concerning RSDs of Youden pair ratios, RSD≤15% values have a proportion exceeding 85% for both green tea and Woolong tea, and the percentage is greater than 87% whether it is for two kinds of SPE cartridges or two kinds of instruments. In terms of Youden pair ratios and the classified statistical analysis of the ruggedness data of parallel samples, the proportion of RSD≤15% values of Youden pair ratios is 8% higher for the TPT cartridge than the ENVI-CARB+PSA cartridge; the proportion of RSD≤15% values of parallel samples is 6.2% higher for the TPT cartridge than the ENVI-CARB+PSA cartridge. Data show no marked differences for two teas and two kinds of instruments. A comparison of the aforementioned aspects finds that good ruggedness was obtained with both SPE cleanup methods, and the results from the TPT cartridge are better than those from the ENVI-CARB+PSA cartridge.

High-Throughput Analytical Techniques for Determination of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea--Part V: A Comparative Study of the Influence of Tea Hydration on the Efficiency of Pesticide Multiresidue Determination Using Three Sample Preparation Methods and GC/MS/MS.

This paper describes a comparative study of the influence of three sample preparation techniques (M1: hydration+oscillating extraction+partial extraction solution hexane partitioning cleanup; M2: hydration+oscillating extraction+overall extraction solution SPE cleanup; and M3: pure acetonitrile homogeneous extraction+overall extraction SPE cleanup) on the determination efficiency of 456 pesticide multiresidues in tea. First, it was discovered from the mathematical correlation equation of 329 pesticide recoveries established and log Kow values that the extraction efficiency of hydration method M1 has obvious correlation with pesticide log Kow, making the extraction efficiency of M1 take the shape of an arc trend line with a certain arc hanging down from both ends of polar pesticides and nonpolar pesticides. Second, regarding the M1 method, the interfering matter after co-extraction increased in large quantities, which markedly lowered the S/N of the target pesticides and method sensitivity, leading to an obvious decrease of the method efficiency. The fortification experiment of the uniform limit 0.010 mg/kg proved that with the M1 hydration method there are 23 pesticides with recoveries between 70 and 120% and RSD<20%, accounting for only 5.0%, while with nonhydration method M3 there are 229 pesticides, making up 50%.

Determination of trace elements in rape honey and its corresponding rape flower and stem by ICP-MS.

The determination of 10 trace elements including Na, Mg, P, K, Ca, Mn, Zn, Rb, Sr and Ba, in rape honey and its corresponding rape flower and stem gathered from nine sampling sites was carried out by inductively coupled plasma mass spectrometry (ICP-MS). The contents of K, P, Ca, Mg and Na were obviously higher than Zn, Rb, Mn, Sr and Ba in rape honey, rape flower and rape stem. For the first five elements, K had the highest content, followed by P, Ca, Mg and Na. However, the order of content for latter five elements was not the same in different matrixes. The contents of K, P and Ca were all higher than 1 000 mg x kg(-1) in rape flower and rape stem, while the contents of P, Ca, Mn, Zn and Rb in rape flower were slightly higher than in rape stem. It can be concluded that rape flower showed slightly higher concentrating ability for trace elements than rape stem. Based on these results, radar chart was firstly applied to research the relationship of 10 elements in rape honey and its corresponding rape flower and stem. The aim of the present work was to study the possibility of using trace elements contents in rape flower to trace the geographical and botanical origin of honey instead of rape honey. It can be found from the radar charts that the stars of rape honey, rape flower and rape stem were similar to each other. This research not only provides the basic data of trace elements in comparative study of rape honey, but also gives scientific basis for tracing the origin of rape honey according to the trace elements in corresponding rape flower that replaces those of rape honey.

High-throughput analytical techniques for multiresidue, multiclass determination of 653 pesticides and chemical pollutants in tea--Part III: Evaluation of the cleanup efficiency of an SPE cartridge newly developed for multiresidues in tea.

A comparative study was conducted over three stages on the cleanup efficiency of SPE cartridge Cleanert TPT, newly developed for multigroups of pesticide residues in tea. In Stage I, different SPE cartridges C18, graphite carbon black (GCB), primary secondary amine (PSA), and amino (NH2) were purchased and combined into 12 different sequences. Through the comparative test on cleanup efficiency of 84 representative pesticides in tea, Envi-Carb GCB + PSA with a good cleanup effect was selected. In Stage II, GC/MS test results from the comparative study of the extraction efficiency of 201 pesticides spiked into green tea and Woolong tea with Cleanert TPT and Envi-Carb + PSA SPE showed that average recoveries fell within 70-110% and RSD <20% for 193 and 184 pesticides, respectively, for green tea, accounting for 96.0 and 91.0% of the total number, respectively. GC/MS/MS test results also found 193 and 184 pesticides, respectively, meeting the recovery and RSD conditions, accounting for 96.0 and 91.5%, respectively, of the total number. For Woolong tea samples, GC/MS results showed that with Cleanert TPT and Envi-Carb + PSA SPE for cleanup, there were 192 and 177 pesticides, respectively, meeting the conditions, accounting for 95.5 and 88.1% of the total number, respectively. GC/MS/MS results demonstrated that there were 195 and 184 pesticides, respectively, meeting the conditions, accounting for 97.0 and 91.5% of the total number, respectively. It was seen that Cleanert TPT was superior to Envi-Carb + PSA in cleanup efficiency, whether for green or Woolong tea samples, or GC/MS or GC/MS/MS determination. In Stage III, 61104 results of the average content value of pesticides and RSD (two teas xtwo Youden pair concentrations x two kinds of SPE cartridges x two instruments x 19 tests x 201 pesticides) were derived from the 19 times stability tests over 3 months by paralleling three samples every 5 days via two instruments with two kinds of SPE cartridges for cleanup, respectively, against Youden Pair samples of the 201 incurred pesticides from green and Woolong teas. The statistical analysis found that detected values from the target pesticides of the incurred Youden pair samples showed no marked differences with cleanup by either Cleanert TPT or Envi-Carb + PSA, whether for green or Woolong tea, or G/IMS or G/IM/IMS. The test results using the two aforementioned kinds of SPE cleanup for above 93% pesticides had a tolerance less than 15%, which testifies that both cartridge cleanups met the requirement for pesticide residue analysis.

High-throughput analytical techniques for determination of residues of 653 multiclass pesticides and chemical pollutants in tea, Part II: comparative study of extraction efficiencies of three sample preparation techniques.

This paper reports a study of the extraction efficiency for the multiresidue pesticides and chemical pollutants in tea with three methods over three stages. Method 1 adopts the Pang et al. approach: the targets were extracted with 1% acetic acid in acetonitrile and cleaned up with a Cleanert TPT SPE cartridge; Method 2 adopts the QuEChERS approach: the targets were cleaned up dispersively with graphitized carbon and primary-secondary amine (PSA) sorbent; Method 3 adopts the relatively commonly used approach of hydration for solid samples, with tea hydrated before being extracted through salting out with acetonitrile and the cleanup procedures identical to those of Method 1. The three stages comprised two phases of comparative tests on spike recoveries of 201 pesticides and chemical pollutants from different teas and a third phase on determination of the content of the 201 pesticides and chemical pollutants from aged tea samples. In stages I and II, test results of the spike recoveries of 201 pesticides and chemical pollutants demonstrated that 91.4% of the pesticide and chemical pollutant recoveries fell within the range of 70-110%, and 93.2% of the pesticides and chemical pollutants had RSD < 15%, with no marked difference obtained by Method 1 and Method 2 regardless of whether it was green tea or woolong tea, or GC/MS or GC/MS/MS was used for analysis. For pigment removal, Method 1 was superior to Method 2; in terms of easy operation, Method 2 outweighed Method 1. However, Method 3 obtained relatively low recoveries, with 94% of pesticide and chemical pollutant recoveries less than 70%, which proved that Method 3 was not applicable to the determination of multiresidue pesticides and chemical pollutants in tea. Stage III made a comparison of Method 1 and Method 2 for the extraction efficiency of pesticides and chemical pollutants in 165-day-aged samples of green and woolong tea. Test results showed that 94% of the pesticide and chemical pollutant content in the aged tea samples was recovered with Method 1, more than 10% higher than with Method 2 (30-50% higher on average). For green tea, 193 (GC/MS/MS) and 197 (GC/MS) pesticides and chemical pollutants accounted for 96.5% (GC/MS/MS) and 98.0% (GC/MS) with Method 1 higher than with Method 2. For woolong tea, 191 (GC/MS/MS) and 194 (GC/MS) pesticides and chemical pollutants accounted for 95% (GC/MS/MS) and 96% (GC/MS/MS) with Method 1, higher than with Method 2, respectively. In other words, there were definite differences in the test results for aged tea samples between Method 1 and Method 2, which suggests that Method 1 was capable of extracting more residual pesticides and chemical pollutants from the precipitated 165-day-aged tea samples. The reason can be traced to the possibility that Method 1 (high-speed homogenizing) has better extraction efficiency than Method 2 (vortex and oscillation). Therefore, Method 1 was chosen as the sample preparation technique for multiresidue pesticide and chemical pollutant analysis in tea.

High-throughput GC/MS and HPLC/MS/MS techniques for the multiclass, multiresidue determination of 653 pesticides and chemical pollutants in tea.

An efficient and sensitive method has been established for simultaneous determination of 653 pesticides in teas by GC/MS and HPLC/MS/MS. The method involved extraction with acetonitrile followed by cleanup using Cleanert-TPT SPE and subsequent identification and quantitation of 490 pesticides by GC/MS and 448 pesticides by HPLC/MS/ MS. The LODs for pesticides determined by GC/MS were between 1.0 and 500 microg/kg, and those determined by HPLC/MS/MS were between 0.03 and 4820 microg/kg. At the low fortification levels of 0.01-100 microg/kg, the average recoveries of 94% of the pesticides determined by GC/MS were between 60 and 120%, 77% of which had an RSD below 20%. For 91% of pesticides determined by HPLC/MS/MS, the average recoveries were between 60 and 120%, 76% of which had an RSD below 20%. The paper also reports a novel SPE column, Cleanert TPT, which comprised graphitized carbon black (PestiCarb), polyamine silica, and amide polystyrene for purifying the tea samples. The results indicated good repeatiblity and reproducibility.

Simultaneous determination of 346 multiresidue pesticides in grapes by PSA-MSPD and GC-MS-SIM.

The article demonstrates a method of simultaneous determination for 352 pesticide residues in grapes using primary-secondary amine (PSA) matrix solid phase dispersion (MSPD) cleanup and gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). Grape samples (15 g) were mixed with 6 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride, and then extracted with acetonitrile (15 mL) and cleaned up with 0.3 g of dispersive PSA. The analytes were determined by GC-MS-SIM. Four injections for one sample were acquired to cover a total of 352 pesticides. The limit of detection (LOD) for the method was 0.0017-0.2667 mg kg(-1), depending on the nature of compounds. The linear correlation coefficient (r) was equal to or greater than 0.95; at low, medium, and high fortification levels, recoveries ranged from 45% to 136% for 352 pesticides, among which the recoveries between 60%-120% accounted for 97%. The pesticides for which the relative standard deviations (RSD) were equal to or below 20% accounted for 95%. A positive of nine varieties of grape samples was detected out, one of which was abtained Changli city, Hebei province, China. Pesticides were identified by the retention time, molecule ions, fragment ions, and the abundance ratio of the selected ions. The analytical method was rugged, quick, cheap and effective, and suitable for the determination of a wide scope of 346 pesticides in grapes.