Evaluation of relevant time-of-flight-MS parameters used in HPLC/MS full-scan screening methods for pesticide residues

An automatic screening method based on HPLC/time-of-flight (TOF)-MS (full scan) was used for the analysis of 103 non-European fruit and vegetable samples after extraction by the quick, easy, cheap, effective, rugged, and safe method. The screening method uses a database that includes 300 pesticides, their fragments, and isotopical signals (910 ions) that identified 210 pesticides in 78 positive samples, with the highest number of detection being nine pesticides/sample. The concentrations of 97 pesticides were <10 microg/kg, 53 were between 10 and 100 microg/kg, and 60 were at a concentration of >100 microg/kg. Several parameters of the automatic screening method were carefully studied to avoid false positives and negatives in the studied samples; these included peak filter (number of chromatographic peak counts) and search criteria (retention time and error window). These parameters were affected by differences in mass accuracy and sensitivity of the two HPLC/TOF-MS systems used with different resolution powers (15 000 and 7500), the capabilities of which for resolving the ions included in the database from the matrix ions were studied in four matrixes, viz., pepper, rice, garlic, and cauliflower. Both of these mass resolutions were found to be satisfactory to resolve interferences from the signals of interest in the studied matrixes.     

气相色谱-质谱法分析蜂蜜中的多种农药残留

开展了蜂蜜中23种农药残留的气相色谱-电子轰击离子源质谱(GC-EI/MS)分析方法的研究,并对其中3种农药的EI/MS碎片离子的断裂机理与结构进行了初步解析。探讨了蜂蜜试样前处理条件的优化与选择。将蜂蜜试样用乙酸乙酯提取剂超声提取、Florisil硅藻土色谱柱净化和正己烷-乙酸乙酯(体积比为7∶3)混合洗脱剂洗脱后,以PCB103为内标物,采用选择离子监测(SIM)方式下的GC-EI/MS分析。当试样的加标浓度为50,100和200 μg/kg时,加标回收率为82%～120%,相对标准偏差小于11.0%。23种农药的检测限都小于10.0 μg/kg,线性范围为10～500 μg/kg,相关系数都大于0.995。此分析方法已成功地应用于蜂蜜中23种痕量农药残留的分析。     

Validation of a gas chromatography/triple quadrupole mass spectrometry based method for the quantification of pesticides in food commodities

A new multiresidue method has been validated in cucumber matrix for the routine analysis of 130 multiclass pesticide residues by gas chromatography/triple quadrupole mass spectrometry. The pesticides were extracted with ethyl acetate. A first identification of the pesticides was based on a tandem mass spectrometric (MS/MS) screening method, which monitors a single transition for each target compound, in less than 12 min. After that, potentially non-negative samples were analyzed again by the MS/MS confirmation/quantification method, which monitors two or three MS/MS transitions for each compound, also in less than 12 min. Performance characteristics, such as trueness, precision, linear range, detection limit (LOD) and quantification limit (LOQ), for each pesticide were calculated. The average recoveries obtained ranged between 70 and 120% at three different fortification levels (25, 200 and 500 microg/kg) with precision, expressed as relative standard deviation (RSD), values lower than 15%. The calculated LOD and LOQ were typically <3.2 and 9.6 microg/kg, respectively. Such limits were much lower than the maximum residue levels (MRLs) established by European legislation. The proposed methodology was applied to the determination of pesticides in real vegetable samples from Almería (Spain).     

Development of a multi-residue screening method for the determination of pesticides in cereals and dry animal feed using gas chromatography-triple quadrupole tandem mass spectrometry

A multi-residue screening method for simultaneous analysis of 122 gas chromatography amenable pesticides in dry matrices such as cereal grain and certain feedingstuffs was developed. The method entails a simple extraction of re-hydrated sample with acetonitrile followed by a dispersive solid phase extraction (dispersive-SPE) clean-up step prior to the final determination by gas chromatography/triple quadrupole tandem mass spectrometry (GC-MS/MS). Due to complexity of analyzed matrices, two MS/MS transitions were set for each pesticide to eliminate the need for re-analysis of potentially positive samples, and provide unequivocal identification of detected pesticides in accordance with recent guidelines, in a single analytical run. Thus, in the developed GC-MS/MS acquisition method, a total of 216 different multiple reactions monitoring (MRM) transitions were monitored in one set of experimental conditions. To evaluate performance of the method, validation experiments were carried out on wheat grain at three spiking levels (0.01, 0.02 and 0.05 mg kg(-1)). Additional recovery tests at 0.05 mg kg(-1) were carried out on several other matrices. The recoveries ranged between 73 and 129% with associated relative standard deviations between 1 and 29% for the majority of pesticides. Limits of detection were less or equal to 0.01 mg kg(-1) for approximately 68% of pesticides. The applicability of the proposed method to detect and quantify pesticide residues has been demonstrated in the analysis of 136 real samples. Additionally, the method was favorably compared with an acetone extraction method (accepted as a reference method by some of European and U.S. authorities) in the analysis of real samples known to contain pesticide residues.     

Determination of pesticides in soy-based infant formula using liquid chromatography with electrospray ionization tandem mass spectrometry

A sensitive method using liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) was developed and validated to quantify and confirm 13 pesticides, including aldicarb sulfoxide, aldicarb sulfone, oxamyl, methomyl, formetanate, 3-hydroxycarbofuran, carbendazim, thiabendazole, aldicarb, propoxur, carbofuran, carbaryl, and methiocarb, in soy-based infant formula. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring of 2 fragment ion transitions to provide a high degree of sensitivity and selectivity for both quantitation and confirmation. Different approaches to constructing calibration curves were compared and discussed to address issues of the extraction efficiency or recovery, and matrix effects. Matrix-matched standard calibration curves with the use of isoprocarb as an internal standard were finally used to achieve the best accuracy of the method. Under most circumstances, recoveries of 13 pesticides, spiked at 5.0, 25.0, and 45.0 microg/kg, were close to 100%. The method detection limits (signal-to-noise ratio > or =3:1; microg/kg) of 13 pesticides were 0.2 for thiabendazole and methiocarb, 0.6 for aldicarb, and 0.1 for the others.     

Determination of three natural pesticides in processed fruit and vegetables using high-performance liquid chromatography/tandem mass spectrometry

This paper describes a method for the sensitive and selective determination of two macrocyclic lactones (abamectin and spinosad) and azadirachtin in apple purée, concentrated lemon juice, tomato purée and canned peas. The general sample extraction-partitioning method for our gas chromatography and liquid chromatography multiresidue methods has been used. The analytical procedure involves an extraction with acetone and liquid-liquid partitioning with ethyl acetate/cyclohexane combined in one step. The extracts are analyzed by liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) without any further clean-up step. The pesticides are separated on a reversed-phase C12 column using a gradient elution. Thirteen simultaneous MS/MS transitions of precursor ions were monitored. Studies at fortification levels of 2.5-10 microg/kg and 25-100 microg/kg gave mean recoveries ranging from 70-100% for all compounds with satisfactory precision (relative standard deviation (RSD) from 3-20%). The excellent selectivity and sensitivity allows quantification and identification of low levels of pesticides in canned peas, tomato and apple purées (limits of quantitation (LOQs) 1-5 microg/kg) and in concentrated lemon juice (LOQs 2-10 microg/kg). The quantification of analytes was carried out using the most sensitive transition for every compound and by 'matrix-matched' standards calibration.     

Determination of pesticides in apples by liquid chromatography with electrospray ionization tandem mass spectrometry and estimation of measurement uncertainty

A liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) method was developed and validated to determine 90 pesticides in apple samples. MS/MS data acquisition was achieved by applying multiple-reaction monitoring of 2 fragment ion transitions to provide a high degree of sensitivity and selectivity for both quantitation and confirmation. Matrix-matched standard calibration curves with the use of isotopically labeled standards (or a chemical analog) as internal standards were used to achieve the best accuracy for the method. Both a conventional method validation procedure and a designed experiment were applied to study the accuracy and precision of the method. A compiled computer program that provided a semiautomated procedure for handling a large number of calculations was used to calculate the overall recovery, intermediate precision, and measurement uncertainty (MU). In general, the overall recoveries from samples spiked at levels of 10, 50, and 80 microg/kg, ranged from 60.8 to 121.1%, intermediate precision was <10%, and MUs were <30%. Poor accuracy and/or repeatability was observed for pyridate and etofenprox. The method limits of detection based on a signal-to-noise ratio of >3 were usually <1 microg/kg (ppb), except those for aldicarb sulfoxide and pyridaphenthion, which were about 5 microg/kg.     

固相萃取-液相色谱-质谱/质谱法同时测定蜂蜜中的多类药物残留

建立了采用固相萃取-液相色谱-质谱/质谱(SPE-LC-MS/MS)对蜂蜜中磺胺类、硝基咪唑类、喹诺酮类、大环内酯类、林可酰胺类和吡喹酮共计6大类54种药物残留同时测定的方法。蜂蜜经磷酸盐缓冲溶液(pH 8)稀释,Oasis HLB固相萃取柱净化后,通过液相色谱-质谱联用技术进行检测(正离子方式,多反应监测模式)。采用同位素稀释内标法或外标法进行定量,线性关系良好,相关系数大于0.992。方法的定量限(LOQ,以信噪比(S/N)大于10计)分别为磺胺类和硝基咪唑类药物1.0 μg/kg,喹诺酮类和林可酰胺类药物2.0 μg/kg,大环内酯类药物3.0 μg/kg,吡喹酮0.3 μg/kg。总体回收率为32.6%～114%,相对标准偏差为1.3%～28.9%。该方法的定量限满足目前国内外药物的最大残留限量要求,可作为蜂蜜中相关药物残留量的筛选检测方法。     

Simultaneous analysis of 260 pesticide residues in agricultural products by gas chromatography/triple quadrupole mass spectrometry

A method for simultaneous analysis of about 260 pesticides by gas chromatography coupled to tandem mass spectrometry (GC/MS/MS) with a triple quadrupole analyzer (QqQ) has been studied. The pesticides were extracted with acetonitrile and cleaned up by a bilayer cartridge. A single injection method was developed for the monitoring of all of the targeted pesticides. Two MS/MS transitions were selected for each analyte using the intensity ratio obtained from them as a confirmatory parameter. By using matrix-matched standards, 260 pesticides could be determined in most matrixes with recoveries of 70-120% and a standard deviation of < or = 20 at 2 different fortification levels of 0.02 and 0.1 microg/g. The developed method was applied to the monitoring of 173 agricultural product samples from the local market. The sensitivities of this method were lower than with most of the selective GC detectors, such as flame photometric or single MS. The selectivity of QqQ gives a very clean chromatogram, making compound identification and confirmation easy. The quick and reliable monitoring was achieved by combination with rapid extraction and cleanup.     

Multi-residue method for the analysis of 101 pesticides and their degradates in food and water samples by liquid chromatography/time-of-flight mass spectrometry

A comprehensive multi-residue method for the chromatographic separation and accurate mass identification of 101 pesticides and their degradation products using liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS) is reported here. Several classes of compounds belonging to different chemical families (triazines, organophosphorous, carbamates, phenylureas, neonicotinoids, etc.) were carefully chosen to cover a wide range of applications in the environmental field. Excellent chromatographic separation was achieved by the use of narrow accurate mass windows (0.05 Da) in a 30 min interval. Accurate mass measurements were always below 2 ppm error for all the pesticides studied. A table compiling the accurate masses for 101 compounds together with the accurate mass of several fragment ions is included. At least the accurate mass for one main fragment ion for each pesticide was obtained to achieve the minimum of identification points according to the 2002/657/EC European Decision, thus fulfilling the EU point system requirement for identification of contaminants in samples. The method was validated with vegetable samples. Calibration curves were linear and covered two orders of magnitude (from 5 to 500 microg/L) for most of the compounds studied. Instrument detection limits (LODs) ranged from 0.04 to 150 microg/kg in green-pepper samples. The methodology was successfully applied to the analysis of vegetable and water samples containing pesticides and their degradation products. This paper serves as a guide for those working in the analytical field of pesticides, as well as a powerful tool for finding non-targets and unknowns in environmental samples that have not been previously included in any of the routine target multi-residue methods.     

Rapid confirmation/quantitation of cocaine and benzoylecgonine in urine utilizing high performance liquid chromatography and tandem mass spectrometry

A rapid, but sensitive and selective method for confirmation and quantitation of benzoylecgonine (BZE) and cocaine (COC) in urine by fast-gradient liquid chromatography/tandem mass spectrometry (LC/MS/MS) is described. The chromatographic separation was performed on a reversed phase column employing fast-gradient techniques. Matrix prepared standards, blanks, and QC's were filtered then aliquots were transferred into a 96 well plate. Injection volumes of 25 microL were made onto the analytical column, with the flow diverted from the atmospheric pressure ionization source for the first 0.5 min of the analysis. Simultaneous multiple reaction monitoring (MRM) of three discrete transitions for each compound were used to identify BZE and COC. Quantitation was achieved utilizing the most prominent parent-daughter transition and internal standard calibration techniques. The coefficients of variation (CV) for the analysis of these drugs ranged from 0.6% to 6.8% at a concentration of 150 ng/mL (n = 155). This method suggests that fast-gradient LC/MS/MS may be suitable for routine confirmation of immunoassay cocaine-positive samples.     

Quantification,confirmation and screening capability of UHPLC coupled to triple quadrupole and hybrid quadrupole time‐of‐flight mass spectrometry in pesticide residue analysis

The potential of three mass spectrometry (MS) analyzers (triple quadrupole, QqQ; time of flight, TOF; and quadrupole time of flight, QTOF) has been investigated and compared for quantification, confirmation and screening purposes in pesticide residue analysis of fruit and vegetable samples. For this purpose, analytical methodology for multiresidue determination of 11 pesticides, taken as a model, has been developed and validated in nine food matrices for the three mass analyzers coupled to ultra high pressure liquid chromatography. In all cases, limits of quantification around 0.01 mg/kg were reached, fulfilling the most restrictive case of baby‐food analysis. Regarding absolute sensitivity, the lower limits of detection were obtained, as expected, for QqQ (100 fg), whereas slightly higher limits (300 fg) were obtained for both TOF and QTOF. Confirmative capacity of each analyzer was studied for each analyte based on the identification points (IPs) criterion, useful for a comprehensive comparison. QTOF mass analyzer showed the highest confirmatory capacity, although QqQ normally led to sufficient number of IPs, even at lower concentration levels. The potential of TOF MS was also investigated for screening purposes. To this aim, around 50 commercial fruits and vegetables samples were analyzed, searching for more than 400 pesticides. TOF MS proved to be an attractive analytical tool for rapid detection and reliable identification of a large number of pesticides thanks to the full spectrum acquisition at accurate mass with satisfactory sensitivity. This process is readily boosted when combined with specialized software packages, together with theoretical exact mass databases. Several pesticides (e.g. carbendazim in citrus and indoxacarb in grape) were detected in the samples. Further unequivocal confirmation of the identity was performed using reference standards and/or QTOF MS/MS experiments. Copyright © 2010 John Wiley & Sons, Ltd.     

超高效液相色谱-四极杆飞行时间质谱快速检测动物饲料中10种违禁精神药物

建立了测定动物饲料中三唑仑、艾司唑仑、硝西泮、地西泮、异丙嗪、氯氮平、唑吡坦、甲硫哒嗪、氯丙嗪和咪达唑仑10种违禁精神药物的超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF-MS)方法。样品经混合溶剂甲醇-0.1 mol/L HCl(9:1, v/v)振荡提取,再用MCX固相萃取柱净化处理后,采用UPLC-Q-TOF-MS分析检测。10种化合物在5～100 μg/L范围内均呈良好的线性关系,线性相关系数均大于0.99。本方法的硝西泮、唑吡坦和甲硫哒嗪的定量限(LOQ,以信噪比为10计)为8 μg/kg,三唑仑、艾司唑仑、地西泮、异丙嗪、氯丙嗪和咪达唑仑为10 μg/kg,氯氮平为20 μg/kg。3个添加水平(LOQ、2LOQ、4LOQ)的回收率试验结果表明,10种化合物的回收率在60.6%～108.5%范围内,相对标准偏差均小于10%。本方法可用于动物饲料中违禁精神药物的准确测定。     

Determination of pesticides in vegetables using large-volume injection column liquid chromatography-electrospray tandem mass spectrometry

Direct injection of a large volume (900 microl) of a sample extract onto a liquid chromatographic (LC) column, LC separation and electrospray tandem mass spectrometric detection were used for the quantitative analysis of a wide polarity range of pesticides in carrots and potatoes. Rapid sample preparation involved extraction of a small amount of sample (2 g) with a small volume of organic solvent (3 ml), clean-up over a filter and dilution of the organic extract with the aqueous LC eluent. The extraction efficiency for the selected pesticides was studied using methanol, acetone and acetonitrile as solvents. Evaluation of the performance of the overall method, using extraction with acetonitrile and detection in the selected-reaction-monitoring mode, showed excellent linearity in the range of 2-100 microg/kg with limits of detection of 0.5-2 microg/kg for both types of vegetable. With relative standard deviations of the MS peak area measurements of less than 6.5% (n=8) the repeatability of the method was fully satisfactory.     

Multiresidue liquid chromatography tandem mass spectrometry determination of 52 non gas chromatography-amenable pesticides and metabolites in different food commodities

A multiresidue method is developed for the screening, quantification and confirmation of 43 pesticides, belonging to different chemical families of insecticides, acaricides, fungicides, herbicides and plant growth regulators, and 9 pesticide metabolites in four fruit and vegetable matrices. Pesticide residues are extracted from the samples with MeOH:H2O (80:20, v/v) 0.1% HCOOH, and then a cleanup step using OASIS HLB SPE cartridges is applied. The SPE eluate is concentrated and the final volume adjusted to 1 mL with MeOH:H2O (10:90, v/v) before injection into LC-MS/MS. Analyses are performed using electrospray ionization (ESI) and triple quadrupole (QqQ) analyzer. The method has been validated based on the SANCO European Guidelines for representative samples that were chosen to study the influence of different matrices: high water content (tomato), high acidic content (lemon), high sugar content (raisin) and high lipidic content (avocado). Special attention has been given to minimize the degradation of some pesticides into their metabolites and the losses observed in the evaporation step. Under the optimized conditions, the recoveries were, with a few exceptions, in the range 70-110% with satisfactory precision (CV < or = 15%). The quantification of analytes was carried out using the most sensitive transition for every compound and by "matrix-matched" standards calibration. The method can be used for the accurate determination of 52 pesticides and metabolites in one single determination step at the 0.01 mg/kg level. Confirmation of residues detected in samples is performed by an independent injection into the LC-MS/MS system by acquiring additional MS/MS transitions to that used for quantification. The acquisition of the highest number of available transitions is suggested for unequivocal confirmation of the analyte.     

Multiresidue determination of pesticides in sediment by ultrasonically assisted extraction and gas chromatography/mass spectrometry

A gas chromatographic/mass spectrometric (GS/MS) method was developed for the multiple determination of pesticides in sediment. The investigated pesticides included 85 compounds, i.e., 13 fungicides, 43 herbicides, and 29 insecticides. The pesticides were extracted from sediment samples by an ultrasonically assisted procedure. The extract was cleaned up by using reversed-phase column chromatography followed by normal-phase column chromatography. A styrene-divinylbenzene copolymer cartridge and a silica gel cartridge were used as the reversed-phase column and the normal-phase column, respectively. The compounds were determined by GC/MS with 2 internal standard compounds. The overall recoveries were 70-105%, and the relative standard deviations ranged from 1.5 to 18%. The minimum detectable concentrations were 2-10 microg/kg. This method was successfully applied to sediment samples from the Shin River in Niigata, Japan. Twenty-five pesticides (6 fungicides, 11 herbicides, and 8 insecticides) were detected in the sediment samples. The concentrations of the detected pesticides ranged from 3 to 69 microg/kg. Herbicides were found May through July; insecticides and fungicides were found July through August, and during July through September, respectively. The presence of pesticides in the river sediment was correlated with the time of pesticide application in the Shin River basin.     

气相色谱-串联质谱法快速筛查测定中药材中144种农药残留

利用气相色谱-串联质谱(GC-MS/MS)检测技术,采用QuEChERS法作为样品前处理方法,建立了能应用于11种中药材中144种农药残留的检测方法。探究了样品前处理过程中提取溶剂、缓冲盐体系、净化剂组成和用量对样品提取、净化等方面的影响,最终确定了用乙腈提取,甲苯复溶,以混合净化剂净化,过有机膜后经GC-MS/MS测定,外标法定量。144种农药在10~2000 μg/kg之间线性关系良好,相关系数(r²)>0.983;除乙酰甲胺磷、灭虫威、西玛津、克菌丹、异狄氏剂、异菌脲外,其余农药的定量限(LOQ)均低于20 μg/kg;在20、50、200 μg/kg的添加水平下,除乙酰甲胺磷、艾氏剂和双甲脒回收率偏低外,其余141种农药的平均回收率在74.3%~111.8%之间,相对标准偏差(RSD)为0.5%~14.6%。与已有的标准方法对比,此方法不仅检测结果一致,而且高效、快速,准确性好,灵敏度高,适用于中药材中144种农药残留的快速筛查与定量分析。     

Evaluation of two-dimensional gas chromatography-time-of-flight mass spectrometry for the determination of multiple pesticide residues in fruit

In recent years, comprehensive two-dimensional gas chromatography (GC x GC) has attained increasing attention for its outstanding separation potential and capability to solve demanding analytical tasks. Trace level analysis of pesticides residues in complex food matrices represents such a demanding task. For some commodities, such as baby food, the requirements on method detection limits are very strict and the unambiguous confirmation of the pesticide presence based on mass spectrometric detection is required. In this work, GC x GC coupled to time-of-flight mass spectrometry (TOF MS) has been evaluated for the determination of pesticides residues in fruit samples. Twenty modern pesticides with a broad range of physico-chemical properties were analysed in apple and peach samples. It has been demonstrated that the application of comprehensive two-dimensional gas chromatography brings distinct advantages such as enhanced separation of target pesticides from matrix co-extracts as well as their improved detectability. The limits of detection of the pesticides comprised in the study (determined at S/N = 5) ranged from 0.2 to 30 pg, injected with the exception of the last eluted deltamethrin, for which 100 pg could be detected. When compared to one-dimentional GC-TOF MS analysis under essentially the same conditions the detectability enhancement was 1.5-50-fold. Full mass spectral information by time-of-flight mass spectrometry and the deconvolution capability of the dedicated software allowed for reliable identification of most pesticides at levels below 0.01 mg/kg (< 10 pg injected) in fruit. Performance characteristics of the GC x GC-TOF MS method, such as linearity of calibration curves, repeatability of (summed) peak areas, as well as repeatability of first and second dimension retention times, were shown to fully satisfy the requirements for trace level analysis of the pesticide residues in food.     

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.     

FastTrack to supercritical fluid chromatographic purification: Implementation of a walk-up analytical supercritical fluid chromatography/mass spectrometry screening system in the medicinal chemistry laboratory

Medicinal chemists often depend on analytical instrumentation for reaction monitoring and product confirmation at all stages of pharmaceutical discovery and development. To obtain pure compounds for biological assays, the removal of side products and final compounds through purification is often necessary. Prior to purification, chemists often utilize open-access analytical LC/MS instruments because mass confirmation is fast and reliable, and the chromatographic separation of most sample constituents is sufficient. Supercritical fluid chromatography (SFC) is often used as an orthogonal technique to HPLC or when isolation of the free base of a compound is desired. In laboratories where SFC is the predominant technique for analysis and purification of compounds, a reasonable approach for quickly determining suitable purification conditions is to screen the sample against different columns. This can be a bottleneck to the purification process. To commission SFC for open-access use, a walk-up analytical SFC/MS screening system was implemented in the medicinal chemistry laboratory. Each sample is automatically screened through six column/method conditions, and on-demand data processing occurs for the chromatographers after each screening method is complete. This paper highlights the “FastTrack” approach to expediting samples through purification.