Use of liquid chromatography quadrupole time-of-flight mass spectrometry in the elucidation of transformation products and metabolites of pesticides. Diazinon as a case study

Liquid chromatography (LC) coupled to hybrid quadrupole time-of-flight (QTOF) mass spectrometry (MS) is a useful analytical tool in the elucidation and confirmation of transformation products (TPs)/metabolites of pesticides with a wide range of polarity, in both environmental and biological samples. Firstly, the versatility of LC allows the determination of very distinct TPs/metabolites as chromatographic conditions can be easily changed and optimized depending on the analytical problem. Secondly, the mass accuracy provided by the TOF analyser allows the assignment of a highly probable empirical formula for each compound and the differentiation between nominal isobaric compounds. Finally, the possibility of performing MS/MS spectra with accurate mass measurements can been used for the final characterization of the TPs/metabolites detected and for the differentiation of isomeric compounds. In this study, the insecticide diazinon was used as model compound, and its photodegradation and metabolism have been investigated by LC-QTOF-MS. On one hand, environmental spiked water was irradiated with a mercury lamp for 9 days, sampling 3-mL aliquots approximately every 12 h. On the other hand, both in vitro and in vivo metabolism experiments were carried out with different substrate concentrations and incubation times. After centrifugation, and protein precipitation in the in vitro and in vivo studies, 50-μL aliquots of both environmental and biological samples were directly injected into the LC electrospray ionization QTOF system. The most important transformation processes were found to be hydrolysis of the ester moiety, hydroxylation in the aromatic ring or in one of the alkylic groups, oxidation of the sulfur atom on the P=S cleavage or a combination of these processes, with the highest number of compounds being found in the photodegradation study. Very polar compounds, such as diethyl phosphate and diethyl thiophosphate, were detected after direct injection of the aqueous sample, which was feasible owing to the characteristics of the LC. In MS mode, mass errors were below 3 mDa, leading to an empirical formula for each compound. MS/MS spectra with accurate mass were used for the final elucidation of the compounds detected.     

Quantitative liquid chromatography/time-of-flight mass spectrometry

Over the last decade, time-of-flight (TOF) instruments have increasingly been used as quantitation tools. In addition, because of their high resolving power, they can be used for verification of empirical formulas. Historically, TOF instruments have had limited quantitation capabilities because of their narrow dynamic range. However, recent advances have improved these limitations. This review covers the rationale for using TOF for LC detection, and describes the many methods currently in the literature for the quantitation of pharmaceuticals, environmental pollutants, explosives and many phytochemicals.     

Ultra-high capacity liquid chromatography chip/quadrupole time-of-flight mass spectrometry for pharmaceutical analysis

Nanoflow liquid chromatography/mass spectrometry (nano-LC/MS) has attracted increasing interest in virtue of high sensitivity, low sample consumption, and minimal matrix effect. In this work a HPLC-Chip/quadrupole time-of-flight (Q-TOF) MS device with a new ultra-high capacity small molecule chip (UHC-Chip) which features a 500 nL enrichment column and a 150 mm × 75 μm analytical column, was evaluated with a drug mixture covering a wide range of polarities. Excellent chromatographic precision with 0.1-0.5% RSD for retention time and 1.7-9.0% RSD for peak area, low limit of detection, good chip-to-chip reproducibility and linearity were obtained by using this UHC-Chip. Compared with the standard HPLC-Chip with 40 nL trapping column, the UHC-Chip showed higher enrichment capability and hence gave a higher response in signal detection. Additionally, 4-30 times increase in sensitivity was obtained compared with conventional LC/MS, which indicated that UHC-Chip/MS was a valuable tool for the quantitative analysis of low level impurities and degradation products in pharmaceuticals. Moreover, satisfactory results obtained from trace drug analysis of serum samples further proved its practicality and potential for use in drug testing and development.     

Application of liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS) in the environmental analysis

This paper gives an overview of the potentials of liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QqTOF) in the environmental analysis. Examples of applications of QqTOF instruments for target analysis of pharmaceuticals and pesticides are presented and discussed, as well as applications aimed on the identification of unknown compounds present in environmental waters or on the elucidation of structures of biodegradation and photodegradation products. Specific issues such as uncertainty of mass measurement and quantitative performances are discussed in details.     

Screening of antibiotics in surface and wastewater samples by ultra-high-pressure liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry

The potential of ultra-high-pressure liquid chromatography (UHPLC) coupled to hybrid quadrupole time-of-flight mass spectrometry (QTOF–MS) for the screening and confirmation of antibiotics in water samples is illustrated in this paper. UHPLC presents several advantages over conventional liquid chromatography as it generates narrow peaks (increasing peak height and improving sensitivity) and reduces chromatographic runs. Regarding QTOF–MS, its increased mass resolution, high sensitivity in full-spectrum acquisition mode and mass accuracy, in both MS and MS/MS modes, make this technique ideal for the detection and reliable confirmation of organic contaminants in environmental samples. After a solid-phase extraction using Oasis HLB cartridges, UHPLC–QTOF–MS has been applied in this work to several types of water samples (surface water and influent and effluent wastewaters). Several antibiotics were found in the samples, such as ofloxacin, ciprofloxacin, clarythromycin or erythromycin, among others. Moreover, the full spectrum data provided by TOF–MS acquisition has enabled searching for many other pharmaceuticals that could be present in the samples in a “post-target” way. This approach has allowed the detection and confirmation of paracetamol, omeprazole and codeine, among others. UPLC–QTOF–MS has been shown as an attractive and efficient hyphenated technique for the rapid detection and confirmation of pharmaceuticals in water with very little sample handling.     

Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry

A novel analytical approach has been developed and evaluated for the quantitative analysis of a selected group of widely used pesticides (dimethoate, simazine, atrazine, diuron, terbuthylazine, methyl-parathion, methyl-pirimiphos, endosulfan I, endosulfan II, endosulfan sulphate, cypermethrin and deltamethrin), which can be found at trace levels in olive oil and olives. The proposed methodology is based on matrix solid-phase dispersion (MSPD), (with a preliminary liquid-liquid extraction in olive oil samples) using aminopropyl as sorbent material with a clean-up performed in the elution step with Florisil, followed by mass spectrometric identification and quantitation of the selected pesticides using both gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode and liquid chromatography tandem mass spectrometry (LC-MS-MS) in positive ionization mode. The recoveries obtained (with mean values between 85 and 115% (obtained at different fortification levels) with RSD values below 10% in most cases, confirm the usefulness of the proposed methodology for the analyses of these kind of complex samples with a high fat content. Moreover, the obtained detection limits, which were below 5 microg kg(-1) by LC-MS analyses and ranged from 10 to 60 microg kg(-1) by GC-MS meet the requirements established by the olive oil pesticide regulatory programs. The method was satisfactorily applied to different olives and olive oil samples.     

Determination of pesticides in water samples by solid phase extraction and gas chromatography tandem mass spectrometry

A multiresidue method for the determination of more than 80 pesticides in water has been developed and validated. The proposed method is based on SPE followed by GC coupled to MS/MS. Different variables affecting SPE procedure, such as cartridges, sample volume and solvents were studied, and mass spectrometric conditions were optimised in order to increase selectivity and sensitivity. Calibration curves were linear over the range of 0.03-0.5 microg/L. Recoveries were in the range of 70-110% and repeatability was below 20% for the lowest calibration point. LODs ranged from 0.001 to 0.025 microg/L and LOQs from 0.003 to 0.076 microg/L. Finally, the method was successfully applied to the analysis of water samples from southeast of Spain.     

Headspace solid phase microextraction in the determination of pesticides in water samples from the Okavango Delta with gas chromatography-electron capture detection and time-of-flight mass spectrometry

Headspace solid phase microextraction (HS-SPME) was optimized for the analysis of pesticides with gas chromatography electron capture detection (GC-ECD) and high-resolution mass spectrometry. Factors influencing the extraction efficiency such as fiber type, extraction mode and temperature, effect of ionic strength, stirring and extraction time were evaluated. The lowest pesticide concentrations that could be detected in spiked aliquots after HS-SPME–GC-ECD ranged from 0.0005 to 0.0032 μg L^{− 1}. Consequently hexachlorobenzene, trans-chlordane, 4,4′-DDD and 4,4′-DDE were detected in water samples after HS-SPME at concentrations ranging from 2.4 to 61.4 μg L^{− 1} that are much higher than the 0.1 μg L^{− 1} maximum limit of individual organochlorine pesticides in drinking water set by the European Community Directive. The same samples were cleaned with ISOLUTE C₁₈ SPE sorbent with an optimal acetone/n-hexane (1:1 v/v) mixture for the elution of analytes. No pesticides were detected after SPE clean-up and pre-concentration. Precision for both methods was satisfactory with relative standard deviations less than 20%. This work demonstrated the superiority of HS-SPME as a sample clean-up and pre-concentration technique for pesticides in water samples as well as the need to identify and control point sources of pesticides.     

超高效液相色谱/高分辨飞行时间质谱法同时检测乳制品中19种抗生素

利用超高效液相色谱/高分辨飞行时间质谱结合数据库建立了乳制品中19种抗生素的分析方法。样品依次经过乙腈和酸化乙腈处理后,冷冻离心浓缩,经超高效液相色谱分离,正离子扫描模式下,在10 min内对19种抗生素进行分离和检测,质量浓度在10～500或15～1000 μg/L范围内具有良好的线性关系,检出限为3～5 μg/L,平均回收率为68.4%～96.7%。加标样品的筛查结果表明,保留时间偏差不大于0.1 min,质量偏差小于5 mDa,同位素峰形匹配度不低于87.4%, 19种加标抗生素被全部检测出来,且大部分抗生素获得很高的鉴定评分。对购自本地超市的40余份乳制品进行了筛查分析,未检出阳性样品。该分析方法具有前处理简单、分析速度快、灵敏度高、质量精确度高的特点,可应用于乳制品中抗生素的快速筛查。     

Screening for pharmaceutical transformation products formed in river sediment by combining ultrahigh performance liquid chromatography/high resolution mass spectrometry with a rapid data-processing method

While the occurrence of pharmaceuticals in the aquatic environment has been extensively investigated, their environmental fate is less thoroughly explored. Scarce information on their transformation pathways and transformation products (TPs) limits conventional target analytical approaches. In this study, samples from water/sediment tests were analyzed by ultrahigh performance liquid chromatography interfaced with quadrupole time-of-flight mass spectrometry (UHPLC/QToF-MS). A data processing method based on peak detection, time-trend filtration and structure assignment was established to provide an efficient way for identifying the key TPs in terms of persistence; all software used for the individual steps of this method is freely available. The accurate mass and meaningful time-trends were major contributors in facilitating the isolation of plausible TP peaks. In total, 16 TPs from 9 parent pharmaceuticals were identified. Eleven out of the 16 TPs were confirmed by corresponding reference standards; no standards were available for the remaining TPs. For additional 6 potential TPs, a molecular formula was suggested but no additional structural information could be generated. Among the TPs identified in the water/sediment tests, carbamazepine-10,11-epoxide (parent: carbamazepine), saluamine (parent: furosemide), chlorothiazide and 4-amino-6-chloro-1,3-benzenedisulfonamide (parent of both: hydrochlorothiazide), and 1-naphthol (parent: propranolol) accumulated over the entire incubation period of 35 days.     

Detecting trace pesticides in real time using single particle aerosol mass spectrometry

Pesticides are toxic substances and may cause unintentional harm if improperly used. The ubiquitous nature of pesticides, with frequent use in agriculture and the household, and the potential for harm that pesticides pose to non-target organisms such as wildlife, humans, and pets, demonstrate the need for rapid and effective detection and identification of these compounds. In this study, single particle aerosol mass spectrometry (SPAMS) was used to rapidly detect compounds from four classes of pesticides commonly used in agricultural and household applications. These include permethrin (pyrethroid class), malathion and dichlorvos (organophosphate class), imidacloprid (chloronicotinyl class), and carbaryl (carbamate class). Analytical standards of each compound were diluted and aerosolized using a nebulizer to create particles for analysis in the SPAMS instrument. The resultant dual-polarity time-of-flight mass spectra were then analyzed to identify the characteristic peaks of the compound in each sample. In addition, samples of commercial products containing pesticides, a commercial insecticide spray, containing permethrin, and a canine flea collar, containing carbaryl, were analyzed in their original form using SPAMS without any significant sample preparation. The characteristic mass spectral peaks of the active pesticides in these samples were identified using the mass spectra obtained earlier from the pesticide analytical standards. By successfully identifying pesticides in analytical standards and in commercial products, it is demonstrated herein that the SPAMS system may be capable of pesticide detection in numerous environmental and agricultural situations.     

Investigating the presence of pesticide transformation products in water by using liquid chromatography-mass spectrometry with different mass analyzers

Many pesticide transformation products (TPs) can reach environmental waters as a consequence of their normally having a higher polarity than their parent pesticides. This makes the development of analytical methodology for reliable identification and subsequent quantification at the sub-microgram per liter levels necessary, as required under current legislation. In this paper we report the photodegradation of several pesticides frequently detected in environmental waters from the Spanish Mediterranean region using the high-resolution and exact-mass capabilities of hybrid quadrupole time-of-flight mass spectrometry (QTOF MS) hyphenated to liquid chromatography (LC). Once the main photodegradation/hydrolysis products formed in aqueous media were identified, analytical methodology for their simultaneous quantification and reliable identification in real water samples was developed using on-line solid-phase extraction (SPE)-LC-tandem MS with a triple-quadrupole (QqQ) analyzer. The methodology was validated in both ground and surface water samples spiked at the limit of quantification (LOQ) and 10 x LOQ levels, i.e. 50 and 500 ng/l, obtaining satisfactory recoveries and precision for all compounds. Subsequent analysis of ground and surface water samples resulted in the detection of a number of TPs higher than parent pesticides. Additionally, several soil-interstitial water samples collected from the unsaturated zone were analyzed to explore the degradation/transformation of some pesticides in the field using experimental plots equipped with lisimeters. Several TPs were found in these samples, with most of them having also been detected in ground and surface water from the same area. This paper illustrates the extraordinary potential of LC-MS(/MS) with QTOF and QqQ analyzers for qualitative/structural and quantitative analysis, respectively, offering analytical chemists one of the most powerful tools available at present to investigate the presence of pesticide TPs in water.     

Screening and identification of multi-component in Qingkailing injection using combination of liquid chromatography/time-of-flight mass spectrometry and liquid chromatography/ion trap mass spectrometry

An approach for screening and identification of multi-component in complex traditional Chinese medicine systems with a combinative LC/MS (MSⁿ) technique was described in this paper. The chemical profile of Qingkailing injection, a well-known traditional Chinese formula in China, was studied using the established method as for an application. Benefit from combining the accurate mass measurement of LC/TOF-MS to generate elemental compositions and the complementary multilevel structural information provided by LC/ion trap MSⁿ, 33 components in Qingkailing injection were identified in all. The three isomers of chlorogenic acid, isochlorogenic acid and neochlorogenic acid which are derived from Flos Lonicerae, one of the medicinal materials in Qingkailing, were differentiated by verifying their MS³ fragmentation data. All the components identified were surveyed and classified according to their medicinal materials derivation. This study is expected to provide an effective and reliable pattern for comprehensive and systematic characterization of the complex traditional Chinese medicine systems.     

Identification and quantitative analysis of the chemical constituents of Gandouling tablets using ultra-high-performance liquid chromatography with quadrupole time-of-flight mass spectrometry

Gandouling tablets are used in a clinical agent for the treatment of hepatocellular degeneration; however, their chemical constituents have not been elucidated. Here, we screened and identified the chemical constituents of Gandouling tablets using ultra-high-performance liquid chromatography (UHPLC)-quadrupole time of flight/mass spectrometry. A method for the quality evaluation of Gandouling tablets was developed by combining the UHPLC fingerprints and the simultaneous quantitative analysis of multiple active ingredients. For fingerprint analysis, 20 shared peaks were identified to assess the similarities among the 10 batches of Gandouling tablets and the similarity was >0.9. The levels of nine representative active ingredients were simultaneously determined to ensure consistency in quality. A total of 99 chemical components were identified, including 18 alkaloids, 20 anthraquinones, 13 flavonoids, 11 phenolic acids, 9 polyphenols, 7 phenanthrenes, 5 sesquiterpenes, 3 curcuminoids, 2 lignans, 2 isoflavones, 2 dianthranones, and 7 other components. The retention times, molecular formulae, and secondary fragmentation information of these compounds were analyzed, and the cleavage pathways and characteristic fragments of some of the representative compounds were elucidated. This systematic analysis used to identify the chemical components of Gandouling tablets lays the foundation for its further quality control and research on their pharmacodynamic substances.     

Discovering metabolites of post-harvest fungicides in citrus with liquid chromatography/time-of-flight mass spectrometry and ion trap tandem mass spectrometry

In this study, we benefit from the combination of liquid chromatography (LC)/time-of-flight (TOF) MS accurate mass measurements to generate elemental compositions of ions and LC/ion trap multiple MS (MSn) providing complementary structural information, which is useful for the elucidation of unknown organic compounds at trace levels in complex food extracts. We have applied this approach to investigate different citrus fruits extracts, and we have identified two post-harvest fungicides (imazalil and prochloraz), the main degradation product of imazalil ([M + H]+, m/z 257) and a non-previously reported prochloraz degradation product ([M + H]+, m/z 282). The database-mediated identification of the parent compounds was based on the generated elemental composition obtained from accurate mass measurements and additional qualitative information from the high resolution chlorine isotopic clusters of both the protonated molecules (imazalil, [M + H]+ 297.0556, <0.1 ppm error, 2-Cl; prochloraz, [M + H]+ 376.0381, 1.9 ppm error, 3-Cl) and their characteristic fragments ions (imazalil: m/z 255 and 159; prochloraz: m/z 308 and 266). The correlation between the structural information provided by ion trap MS/MS fragmentation pathways of the parent species and the TOF accurate mass elemental composition data of the degradation products were the key to elucidate the structures of the degradation products of both post-harvest fungicides. Finally, where standards were not available (prochloraz), further confirmation was obtained by synthesizing the proposed degradation product by acid hydrolysis of the parent standard and confirmation by LC/TOF-MS.     

Critical review of the application of liquid chromatography/mass spectrometry to the determination of pesticide residues in biological samples

A critical review is made on the use of hyphenated liquid chromatography/mass spectrometry (LC–MS) for the identification and quantification of pesticides and their metabolites in human biosamples (whole blood, plasma, serum and urine). The first applications of LC–MS in this field began in the early 1990s. Since then, increasing interest has been shown in applying this powerful technique, with most applications dealing with the determination of a variety of chemically diverse metabolites in urine. The use of different LC–MS interfaces and mass spectral detection modes are discussed. Special attention is given to tandem mass spectrometry (MS/MS) due to its inherent advantages of increased sensitivity and selectivity, as well as its advantages for identification and confirmation of analytes in samples. Quantification can be severely affected by matrix effects, the most common being inhibition of the ionisation of analytes in the mass spectrometer, which leads to unacceptable errors if no correction is made. Different approaches can be employed to minimise this undesirable matrix effect, the preferred being the use of labelled internal standards (when available) in isotope dilution methods or the application of an efficient clean-up, performed off-line or automated on-line. Adequate criteria for confirming the identities of residues detected are required in order to avoid false positives. The criterion most commonly used with a triple quadrupole instrument is the monitoring of two MS/MS transitions together with the ion abundance ratio. TOF mass analysers are seldom used in pesticide residue analysis despite their improved resolution and mass accuracy characteristics, which makes them very suitable for confirmation purposes. The main reasons for the relative unpopularity of TOF MS in residue analysis are its limited sensitivity and its high acquisition cost. In this paper, we present a critical assessment on current techniques, trends and future developments, and give illustrative examples to point out the main characteristics of LC–MS for pesticide residue analysis in biological fluids.     

Direct determination of acrylamide in food by gas chromatography-high-resolution time-of-flight mass spectrometry

Simple and rapid gas chromatographic (GC) method employing a high-resolution time-of-flight mass analyzer that enables direct analysis (no derivatization) of acrylamide in various heat-processed foodstuffs has been developed and validated. Co-isolation of acrylamide precursors such as sugars and asparagine, constituting the risk of results overestimation due to additional formation of analyte in hot GC injector, is avoided by the extraction with n-propanol followed by solvent exchange to acetonitrile (MeCN). Introduction of a novel purification strategy, dispersive solid phase extraction, based on addition of primary-secondary amine (PSA) sorbent into deffated extract in MeCN, provides a significant reduction of some abundant matrix co-extracts (mainly free fatty acids). Isotope dilution technique (d₃-acrylamide as an internal standard) is employed for compensation of potential target analyte losses and/or matrix-inducted chromatographic response enhancement. Limits of quantifications (LOQs) ranged between 15 and 40 μg kg⁻¹ and recoveries were between 97 and 108% depending on the examined food matrix. The repeatability of measurements (expressed as relative standard deviation, R.S.D.) was as low as 1.9% for potato crisps containing acrylamide at a level of 1 mg kg⁻¹. Slightly higher values (R.S.D. < 4.0%) were achieved for breakfast cereals and crisp bread with approximately 10 times lower content of this processing contaminant. Trueness of results generated by this new method was demonstrated via FAPAS^® (Food Analysis Performance Assessment Scheme) interlaboratory proficiency tests.     

Gas chromatography coupled to high-resolution time-of-flight mass spectrometry to analyze trace-level organic compounds in the environment, food safety and toxicology

Gas chromatography coupled to high-resolution time-of flight mass spectrometry (GC-HR-TOF-MS) is a powerful analytical technique with excellent capabilities due to its high sensitivity in full-spectrum-acquisition mode together with its resolving power and accurate-mass measurements. These features make this technique very attractive in qualitative analysis, especially for wide-scope screening of a large number of organic contaminants and residues at trace levels.Full-spectrum MS allows data processing, in principle, of an unlimited number of compounds in samples, as no analyte-specific information is required before the injection. Also, as all data remain available, retrospective analysis is always possible without the need to reinject the sample - an important advantage of full-spectrum MS techniques. Despite these advantages, GC-HR-TOF-MS has rarely been applied, so we expect promising results in different applied fields in the years ahead.We discuss in detail the characteristics and the potential of GC-HR-TOF-MS. We describe different analytical strategies from wide-scope target screening to investigation of unknowns in biology, the environment and food safety. Recent instrumental developments (e.g., high-speed analog-to-digital converter or soft ionization sources) and advances in software for processing the huge amount of data available open up new prospects, making GC-TOF-MS one of the most promising techniques to investigate the presence of organic compounds in different fields.     

Multiresidue determination of 160 pesticides in wines employing mixed-mode dispersive-solid phase extraction and gas chromatography-tandem mass spectrometry

A new multiresidue method for the efficient screening, identification and quantification of over 160 pesticides belonging to different chemical classes in red, rose and white wines have been developed. The analysis was based on gas chromatographic-tandem quadrupole mass spectrometric determination (GC-QqQ-MS/MS). An optimization strategy involved the selection of buffering conditions and sorbents for dispersive-solid phase extraction (dispersive-SPE) in order to achieve acceptably high recoveries and reduce co-extractives in the final extracts. As a result, the optimized procedure allowed us to obtain consistent recoveries of the target pesticides including problematic ones such as captan, chlorothalonil, dichlofluanid, folpet and tolylfluanid. The attained recoveries were typically between 80 and 110% (89% on average) with RSD values typically lower than 10% (8% on average) at three spiking levels of 0.01, 0.05 and 0.2 mg kg⁻¹. Linearity was studied in the range between 0.005 and 0.2 mg kg⁻¹ using pesticide standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination (R²) higher than 0.99 for all the pesticides except for desmedipham, thiabendazole and thiamethoxam in pure solvent. The study of the ratio of the slopes obtained in solvent and in matrix provided information about the matrix effects, which was <10%, 10-20% and >20% for 33, 36 and 31% of the studied pesticides, respectively. To improve accuracy, matrix matched standards were always used for calculation of the quantification results. The expanded uncertainties were estimated by using a “top-down” approach as being 17% on average (coverage factor k = 2, confidence level 95%). Finally, the method was used with success to detect and quantify pesticide residues in commercial wines.     

Multiresidue screening of pesticides in Panax Ginseng C. A. Meyer by ultra-high-performance liquid chromatography with quadrupole time-of-flight mass spectrometry

In this study, an efficient screening method based on a modified quick, easy, cheap, effective, rugged, and safe extraction method combined with ultra-high-performance liquid chromatography coupled to tandem quadrupole time-of-flight mass spectrometry was established for the determination of 90 pesticides residues in Panax Ginseng. The accuracy of the method was then verified by analyzing the false positive rate and the screening detection limit in Ginseng. The results revealed that the screening detection limit of 33 of 90 pesticide residues were 0.01 mg·kg⁻¹, 22 species were 0.05 mg·kg⁻¹, 11 species were 0.10 mg·kg⁻¹, 8 species were 0.20 mg·kg⁻¹, and another 16 species were greater than 0.20 mg·kg⁻¹. A total of 73 pesticides were ultimately suitable to be practically applied for rapid analysis of pesticide residues in Ginseng. Finally, the established method was used to analyze the pesticide residues in 35 Ginseng samples available on the market. And the residual of dimethomorph, azoxystrobin, tebuconazole, and pyraclostrobin was relatively severe in Ginseng samples. This work expanded the range of pesticides detected and provided a rapid, effective method for pesticides screening in Ginseng.