Single-laboratory validation of a method for the determination of furan in foods by using static headspace sampling and gas chromatography/mass spectrometry

A headspace gas chromatography/mass spectrometry method was developed and validated in-house for the determination of furan in foods. The method of standard additions with d4-furan as the internal standard was used to quantitate furan. The limit of detection and limit of quantitation (LOQ) values ranged from 0.2 and 0.6 nglg, respectively, in apple juice to 0.9 and 2.9 ng/g, respectively, in peanut butter. Recoveries were obtained at 0.5, 1, 2, and 3 times the LOQ. At 1, 2, and 3 times the LOQ, the recoveries ranged from 89.4 to 108%, and the relative standard deviations ranged from 3.3 to 17.3% for all the matrixes. For apple juice, chicken broth, and infant formula, the averaged coefficients of determination from the linear regression analyses were >0.99 with each food fortified at 0.5, 1, 2, and 3 times the LOQ. The coefficients of determination were >0.99 for green beans and 0.96 for peanut butter with the foods fortified at 1, 2, and 3 times the LOQ. Within-laboratory precision was determined by comparing the amounts of furan found in 18 samples by 2 analysts on different days with different instruments. For most of the foods, the difference between the amounts found by each analyst was <18%. The method was used to conduct a survey of >300 foods. The furan levels found ranged from none detected to 174 ng/g.     

Single-laboratory validation of a method for the determination of furan in foods by using headspace gas chromatography/ mass spectrometry, part 2--low-moisture snack foods

In 2004, a quantitative headspace (HS) gas chromatographic/mass spectrometric method was developed and used to determine furan in approximately 300 foods. This method was modified and validated for the determination of furan in low-moisture snack foods. The modifications include a smaller test portion size and lower HS oven temperature. The limits of detection ranged from 0.4 ng/g in graham crackers to 4.4 ng/g in pretzels. Recoveries from samples fortified at 0.5, 1,2, and 3 times the levels of incurred furan found in the samples ranged from 96 to 102%, and HorRat values showed that the recovery data met the criteria for repeatability. The modified method was shown to be reliable for the determination of furan in foods when test portions were equilibrated for 30 min in a 60 degrees C HS oven. The modified method was used to conduct a survey of furan in 22 low-moisture snack foods. All of the samples were found to contain furan ranging from 3.7 ng/g in graham crackers to 60 ng/g in corn chips. Results from the survey were consistent with results obtained for similar snack foods analyzed by a U.S. Food and Drug Administration field laboratory.     

Simultaneous separation and determination of 20 potential adulterant antigout and antiosteoporosis pharmaceutical compounds in herbal food products using LC with electrospray ionization MS/MS and LC with quadrupole‐time‐of‐flight MS

An analytical method for the simultaneous and reliable determination of 20 antigout and antiosteoporosis pharmaceutical compounds in adulterated health food products was developed using liquid chromatography with electrospray ionization tandem mass spectrometry and liquid chromatography with quadrupole‐time‐of‐flight mass spectrometry. The method was validated through the determination of specificity, linearity, limit of detection, and limit of quantification, method detection limit, method quantitation limit, precision, accuracy, recovery, and stability. The matrix effect was also determined. The validation results of the developed method are as follows: for solid and liquid blank samples, limits of detection ranged from 0.05 to 5.00 ng/mL and limits of quantification ranged from 0.15 to 15.00 ng/mL. Linearity was acceptable, and the correlation coefficients (R²) were ≥0.99 for all target compounds. Both intra and interday precision were less than 9.16% RSD, and accuracies ranged from 95.31 to 116.68%. Mean recoveries for different types of dietary supplements classified as powders, liquids, tablets, and capsules were found to be 80.81 to 117.62% with less than 15.00% relative standard deviation. The stability of the standard mixture solution was less than 11.72% relative standard deviation after 48 h. By the proposed method, the presence of dexamethasone was determined in seized herbal food products at concentrations that ranged from 126 to 215 µg/g.     

顶空气相色谱-质谱法测定婴幼儿食品中的呋喃

通过顶空装置将样品中的呋喃提取出来,以D4-呋喃作为内标物,HP-PLOT Q石英毛细管柱作为分析柱,采用气相色谱分离,质谱定性定量,建立了婴幼儿食品中呋喃的顶空气相色谱-质谱联用分析方法。方法的低浓度工作曲线的线性范围为10～70 ng,高浓度工作曲线的线性范围为50.0～400.0 ng,两条曲线的相关系数均为0.997。方法的定性检出限（S/N≥3）为3.8 ng/g,定量检出限（S/N≥10）为10.0 ng/g。不同基底样品中高低添加浓度的加标回收率为90.0%～98.4%,相对标准偏差均小于10%。     

Analysis of emerging organic contaminants in poultry manure by gas chromatography–tandem mass spectrometry

A multiresidue method was developed for the determination of 19 emerging organic contaminants (pharmaceutical drugs, personal care products, and bisphenol A) in poultry manure. Lyophilized samples of manure were extracted by ultrasound‐assisted matrix solid‐phase dispersion and the extracts were analyzed by gas chromatography with tandem mass spectrometry after derivatization. Analysis of spiked poultry manure samples, at levels ranging from 25 to 150 ng/g, gave satisfactory recovery results for all the compounds, with values from 67 to 106%. The developed procedure provided detection limits that ranged from 0.9 to 2.2 ng/g. Finally, the validated method was applied to poultry manure samples collected from 23 poultry farms in Spain. Salicylic acid was found in most of the samples analyzed at levels up to 2501 ng/g, whereas, methyl paraben, orthophenylphenol, ibuprofen, paracetamol, and carbamazepine were detected at levels up to 250 ng/g. Composting of manure showed an important decrease in the levels of the detected contaminants.     

Simultaneous analysis of 35 specific antihypertensive adulterants in dietary supplements using LC/MS/MS

A sensitive and specific LC/MS/MS method was developed for the simultaneous analysis of 35 compounds used for treating hypertension as adulterants in dietary supplements. The method was validated for specificity, linearity, accuracy, precision, limit of detection, limit of quantitation, stability and recovery. The limit of detection and limit of quantitation ranged from 0.20 to 20.0 and 0.50 to 60.0 ng/g, respectively. The linearity was good (r ² > 0.999), with intra‐ and interday precision levels of 0.43–7.87% and 0.65–9.95% and the intra‐ and interday accuracies of 84.36–115.82% and 83.78–118.69%, respectively. The stability (relative standard deviation) was <14.75%. The mean recovery was 80.81–117.86% (relative standard deviation <10.00%). Ninety‐seven commercial dietary supplements available in South Korea were analyzed. While none contained detectable amounts of the 35 antihypertensive compounds, the developed LC/MS/MS procedure can be used for routine analysis to monitor illegal adulteration in various forms of dietary supplements.     

Simultaneous screening and quantification of aminoglycoside antibiotics in honey using mixed‐mode liquid chromatography with quadrupole time‐of‐flight mass spectroscopy with heated electrospray ionization

An analytical method based on liquid chromatography with quadrupole time‐of‐flight mass spectrometry has been developed for the simultaneous determination of six aminoglycoside antibiotics in honey. The sample pretreatment included extraction with aqueous trichloroacetic acid followed by solid‐phase extraction on Strata‐X polymeric reversed phase cartridges. Liquid chromatography separation was performed on an Obelisc R zwitterionic type mixed‐mode column. An ionBooster™ heated electrospray source was used and showed enhanced ionization efficiency in comparison to a conventional electrospray source. The observed signal enhancement ranged from 3‐ (neomycin) to 16‐fold (gentamicin C1). A data‐dependent mass spectrometry acquisition approach was employed, in which the full mass spectrometry dataset provided quantification and a scheduled precursor list was used to trigger an alternating data‐dependent acquisition of MS² spectra for confirmation purposes. The described method was validated in accordance to CD 2002/657/EC. Decision limit values were in the range 11.2–33.6 ng/g, and satisfactory performance characteristics were obtained for recovery (65–76%), repeatability (3.8–7.3%), and linearity (≥0.995). The method was applied to the analysis of 49 real honey samples from the country of Georgia. Streptomycin was detected in two samples at 117 and 35 ng/g, and gentamicin C1 was detected in one sample at 32 ng/g.     

Simultaneous determination of novel β-lactamase inhibitor WCK 4234 and Meropenem in dog plasma by LC–MS/MS and its application to preclinical pharmacokinetic study

A precise and accurate liquid chromatography–tandem mass spectrometric (LC–MS/MS) bioanalytical method has been developed and validated for the simultaneous quantification of WCK 4234 and meropenem (MEM) in dog plasma. Protein precipitation using acetonitrile was employed as a sample preparation approach. Cefepime was used as an internal standard. The developed method was selective, sensitive (limit of quantification, 0.075 μg/ml for both drugs), accurate (recovery > 90%), precise (CV < 10%) and linear (r² ≥ 0.99, concentration range 0.075–120 μg/ml for both analytes). The developed method was successfully applied for the determination of both drugs in plasma to assess the pharmacokinetics in beagle dogs. WCK 4234 + MEM in a 1:1 ratio at 15 + 15 and 30 + 30 mg/kg doses were administered by the intravenous route. The mean plasma concentration and area under the concentration–time curve of WCK 4234 ranged from 38.3 to 77.4 μg/ml and from 47.8 to 77.1 μg h/ml, respectively, and the values for MEM ranged from 52.2 to 115.3 μg/ml and 70.5 to 133.6 μg h/ml respectively. The elimination half-life of WCK 4234 and MEM was around 0.8 h.     

Experimental strategy of the spectrophotometric approach using freeze-drying for PO43− determination in frozen and chilled chickens in the Saudi Arabia market

Herein, an efficient analytical method based on an extraction protocol was developed and validated for the spectrophotometric detection of phosphate (PO₄^3?) in chilled and frozen chicken samples. The preparation was a very simple sample that included freeze-drying, extraction with acidified amino acids and filtration of the final extract prior to spectrophotometric analysis. FT-IR spectrum of CS1 was confirmed that the selected solvent has successfully extracted PO₄^3? from the chilled chicken sample. Analytical performances were assessed in chilled of one of the merchant species and showed good recoveries with relative standard deviations (RSD) below 2%. The analytical validation parameters of the method in terms of limit of quantification (LOQ) and detection (LOD) were calculated and found to be 0.10 and 0.032 mg/L, respectively. This protocol has been effectively applied to PO₄^3? determination in chicken samples collected from Saudi supermarkets (Northern KSA), and PO₄^3? in all frozen samples was detected at high mg/kg levels ranging from 2.11 × 10⁴ to 2.90 × 10⁴ mg/kg, while in limit levels of PO₄^3? concentration were detected in the chilled samples except chilled sample 1 (CS1), which was 2.22 × 10⁴ mg/kg. The extraction and determination protocol suggested that this developed method could be validated for routine monitoring of PO₄^3? in food quality control laboratories and safety monitoring.     

Determination of Neonicotinoid Pesticides in Propolis with Liquid Chromatography Coupled to Tandem Mass Spectrometry

In this study, a method was developed for the determination of five neonicotinoid pesticides (acetamiprid, clothianidin, imidacloprid, thiacloprid, and thiamethoxam) in propolis. Two sample preparation methods were tested: solid-phase extraction and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The identities of analytes were confirmed using liquid chromatography–tandem mass spectrometry (LC-MS/MS) in the selected reaction monitoring mode. Solid-phase extraction resulted in cleaner extracts; therefore, the SPE-LC-MS/MS method was validated according to the SANTE protocol in triplicate at two spiking levels (10 ng/g and 50 ng/g). The average recoveries of analytes ranged from 61% to 101%, except for clothianidin (10–20%). The LOD ranged from 0.2 ng/g to 4.4 ng/g, whereas the LOQ was in the range of 0.8 ng/g–14.7 ng/g. In order to compensate for the matrix effect, matrix-matched calibration was used. Good accuracy (relative error: 1.9–10.4%) and good linearity (R² > 0.991) were obtained for all compounds. The optimised method was applied to 30 samples: 18 raw propolis and 12 ethanol tinctures. Acetamiprid, imidacloprid, and thiacloprid were detectable in seven samples but were still below the LOQ. This study is the first to report the determination of several neonicotinoid residues in propolis.     

Meropenem and ciprofloxacin in complicated gastric surgery for cancer patients: A simple SPE–UHPLC–PDA method for their determination in human plasma

A simple and rapid ultra‐high‐performance liquid chromatographic (UHPLC) for the simultaneous determination of meropenem and ciprofloxacin in human plasma was developed and validated. All of the analytes were separated in <5 min. A solid‐phase extraction method was applied from sample preparation. Analytical separation was performed on a Poroshell SB C₁₈ column (50 × 2.1 mm, 2.7 μm particle size) with photodiode array (PDA) detection. Meropenem and ciprofloxacin were determined at wavelengths of 300 and 277 nm, respectively. The mobile phase was a mixture of acetonitrile–10 mm ammonium acetate–methanol in gradient elution. The method has been validated for both drugs in gastric surgery for cancer patients. The method showed good linearity with correlation coefficients, r² = 0.994 for the two drugs, as well as high precision (RSD < 10.5% in each case); accuracy ranged from ?5.8 to +6.0%. The limit of quantitation of the two drugs was established at 0.02 and 0.01 μg/mL, respectively. Meropenem, ciprofloxacin and the internal standard were extracted from human plasma with a mean recovery ranging from 92.5 to 98.6%. The method was applied to quantify the drugs dosage in complicated gastric surgery patients.     

Liquid chromatography with tandem mass spectrometry method for the determination of nicotine and minor tobacco alkaloids in electronic cigarette refill liquids and second‐hand generated aerosol

A liquid chromatography with tandem mass spectrometry method for the simultaneous quantification of nicotine and seven minor tobacco alkaloids in both refill liquids for electronic cigarettes and their generated aerosol was developed and validated. The limit of detection and limit of quantification values were 0.3–20.0 and 1.0–31.8 ng/mL, respectively. Within‐laboratory reproducibility was 8.2–14.2% at limit of quantification values and 4.8–12.7% at other concentration levels. Interday recovery was 75.8–116.4%. The method was applied to evaluate the compliance of commercial liquids (n = 95) with their labels and to assess levels of minor alkaloids. Levels of nicotine and its corresponding compounds were also evaluated in generated aerosol. About 47% of samples showed differences above ±10 % of the stated nicotine concentration. About 78% of the “zero nicotine” liquids showed traces in the range of 1.3 ± 0.1–254.0 ± 14.6 μg/mL. Nicotine‐N ′‐oxides, myosmine, and anatabine were the most common minor alkaloids in liquids containing nicotine. Nicotine and N ′‐oxides were detected in all air samples when aerosol was generated from liquids containing nicotine. Nicotine average emissions from electronic cigarette (2.7 ± 0.9 μg/m³) were significantly lower (p < 0.01, t‐test) with respect to conventional cigarette (30.2 ± 1.5 μg/m³).     

Determination of furan levels in coffee using automated solid-phase microextraction and gas chromatography/mass spectrometry

Furan is a 5-member ring chemical with high volatility. Because it is highly volatile, furan levels in foods are not easily determined with accuracy. In this study, an analytical method for furan analysis using an automated solid-phase microextraction system in combination with gas chromatography/mass spectroscopy is described. The performance of the method was demonstrated by the results obtained from a variety of coffees. Furan was detected at part-per-billion levels in coffee. The limit of detection was 0.3 ng/g and limit of quantitation, 0.8 ng/g. The percent recoveries were between 92 and 102.     

Quantitative determination of 43 common drugs and drugs of abuse in human serum by HPLC-MS/MS

An analytical procedure for the simultaneous determination in human serum of 43 common drugs of abuse and their metabolites belonging to the different chemical and toxicological classes of amphetamines, benzodiazepines, dibenzazepines, cocaine, lysergic acid diethylamide, opioids, phencyclidine, tricyclic antidepressants, and zolpidem, using 33 deuterated standards, is presented. The sample treatment was developed to be a very simple protein precipitation and filtration. All analyses were performed with a high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry in positive ionization mode. All analytes were calibrated up to 550 μg/L. The limit of detection ranged from 0.6 ng/mL (EDDP) to 13.7 ng/mL (flunitrazepam). The method has been validated according to the guidelines of the Gesellschaft für Toxikologische und Forensische Chemie, using three multiple reaction mode (MRM) transitions and retention time for positive compound identification, instead of two MRMs, in anticipation of the new guidelines for January 2011.     

Micellar-stabilized room-temperature phosphorimetric determination of the fungicide thiabendazole in canned pineapple samples

A method for the determination of the fungicide thiabendazole (TBZ) by micellar-stabilized room-temperature phosphorescence is described. It does not require any separation step and allows the direct determination of the fungicide in canned pineapple samples. The effect of various experimental conditions is discussed in detail. The analytical curve of thiabendazole gives a linear dynamic range of 23.8–500.0 ng mL^–1 and a detection limit of 23.8 ng mL^–1. Recoveries of 103.9 and 89.2% for syrup and canned pineapple pulp, respectively, were obtained for 250 ng mL^–1 thiabendazole. Received: 30 April 1997 / Revised: 18 July 1997 / Accepted: 23 July 1997     

Determination of polyfluoroalkyl phosphoric acid diesters, perfluoroalkyl phosphonic acids, perfluoroalkyl phosphinic acids, perfluoroalkyl carboxylic acids, and perfluoroalkane sulfonic acids in lake trout from the Great Lakes region

A comprehensive method to extract perfluoroalkyl carboxylic acids, perfluoroalkane sulfonic acids, perfluoroalkyl phosphonic acids, perfluoroalkyl phosphinic acids, and polyfluoroalkyl phosphoric acid diesters simultaneously from fish samples has been developed. The recoveries of target compounds ranged from 78?% to 121?%. The new method was used to analyze lake trout (Salvelinus namaycush) from the Great Lakes region. The results showed that the total perfluoroalkane sulfonate concentrations ranged from 0.1 to 145?ng/g (wet weight) with perfluorooctane sulfonate (PFOS) as the dominant contaminant. Concentrations in fish between lakes were in the order of Lakes Ontario ≈ Erie > Huron > Superior ≈ Nipigon. The total perfluoroalkyl carboxylic acid concentrations ranged from 0.2 to 18.2?ng/g wet weight. The aggregate mean perfluorooctanoic acid (PFOA) concentration in fish across all lakes was 0.045?±?0.023?ng/g. Mean concentrations of PFOA were not significantly different (p?>?0.1) among the five lakes. Perfluoroalkyl phosphinic acids were detected in lake trout from Lake Ontario, Lake Erie, and Lake Huron with concentration ranging from non-detect (ND) to 0.032?ng/g. Polyfluoroalkyl phosphoric acid diesters were detected only in lake trout from Lake Huron, at levels similar to perfluorooctanoic acid.     

Assessment of the occurrence and distribution of pharmaceuticals in a Mediterranean wetland (L'Albufera, Valencia, Spain) by LC-MS/MS

The distribution of 17 pharmaceuticals between water and the solid phase (sediments and soils) was studied by utilizing solid-phase extraction (SPE) and liquid chromatography?Ctandem mass spectrometry (LC-MS/MS). Two extraction procedures for soils and sediments, prior to the SPE, one based on pressurized liquid extraction (PLE) with hot water and the other on methanol/water ultrasonic extraction, were compared. Absolute recoveries were 71.2?C99.3% [relative standard deviation (RSD) <21.4%)] for water, and the method detection limits (MDLs) ranged from 0.3 to 10?ng?L^?1. Recoveries were 35.4?C105.3% (RSDs <19.1%) and 42.1?C97.8% (RSDs <14%) for soil and sediment samples, respectively, using PLE and 20.2?C86.5% (RSDs <25.1%) and 30.3?C97.4% (RSDs <19.1%) using ultrasonic extraction. Fifteen of the 17 pharmaceuticals were present in the L??Albufera water at concentrations up to 17???g?L^?1. Oxytetracycline and tetracycline were not detected. In sediments, only tetracycline, norfloxacin and diclofenac were not found. The other studied pharmaceuticals were present in the range from less than the method quantification limit (MQL) to 35.83?ng?g^?1. Among the 17 target compounds, ofloxacin, ciprofloxacin, norfloxacin, trimethoprim, clofibric acid and diclofenac were not detected in soil samples. The average concentrations ranged from less than the MQL for ibuprofen to 34.91?ng?g^?1 for tetracycline. These results indicate that pharmaceuticals could survive the wastewater treatment processes, which could lead to their dissemination in water environments.     

Folate analysis in foods by UPLC-MS/MS: development and validation of a novel, high throughput quantitative assay; folate levels determined in Australian fortified breads

An ultra-performance liquid chromatography-tandem mass spectrometry method was developed, optimised and validated for the quantification of synthetic folic acid (FA), also called pteroyl-l-glutamic acid or vitamin B9 and naturally occurring 5-methyltetrahydrofolate (5-MTHF) found in folate-fortified breads. Optimised sample preparation prior to analysis involved addition of ¹³C₅ labelled internal standards, treatments with α-amylase and rat serum, solid-phase extraction using aromatic-selective cartridges and ultra-filtration. Analytes were separated on a Waters ACQUITY HSS T3 column during a 6-min run and analysed by positive ion electrospray selected reaction monitoring MS/MS. Standard calibration curves for the two analytes were linear over the range of 0.018–14 μg FA/g of fresh bread (r ² = 0.997) and 9.3–900 ng 5-MTHF/g of fresh bread (r ² = 0.999). The absolute recoveries were 90% and 76% for FA and 5-MTHF, respectively. Intra-day coefficients of variation were 3% for FA and 18% for 5-MTHF. The limit of detection was 9.0 ng/g for FA and 4.3 ng/g for 5-MTHF, determined using pre-extracted tapioca starch as the blank matrix. The assay is rugged, fast, accurate and sensitive, applicable to a variety of food matrices and is capable of the detection and quantification of the naturally occurring low levels of 5-MTHF in wheat breads. The findings of this study revealed that the FA range in Australian fortified breads was 79–110 μg/100 g of fresh bread and suggest that the flour may not have the mandated FA fortification level (200–300 μg/100 g of flour), though this cannot be determined conclusively from experimental bread data alone, as variable baking losses have been documented by other authors.     

Simultaneous quantification of buprenorphine,norbuprenorphine, buprenorphine glucuronide,and norbuprenorphine glucuronide in human placenta by liquid chromatography mass spectrometry

A LCMS method was developed and validated for the determination of buprenorphine (BUP), norbuprenorphine (NBUP), buprenorphine glucuronide (BUP-Gluc), and norbuprenorphine glucuronide (NBUP-Gluc) in placenta. Quantification was achieved by selected ion monitoring of m/z 468.4 (BUP), 414.3 (NBUP), 644.4 (BUP-Gluc), and 590 (NBUP-Gluc). BUP and NBUP were identified monitoring MS² fragments m/z 396, 414 and 426 for BUP, and 340, 364 and 382 for NBUP, and glucuronide conjugates monitoring MS³ fragments m/z 396 and 414 for BUP-Gluc, and 340 and 382 for NBUP-Gluc. Linearity was 1–50 ng/g. Intra-day, inter-day and total assay imprecision (% RSD) were <13.4%, and analytical recoveries were 96.2–113.1%. Extraction efficiencies ranged from 40.7–68%, process efficiencies 38.8–70.5%, and matrix effect 1.3–15.4%. Limits of detection were 0.8 ng/g for all compounds. An authentic placenta from an opioid-dependent pregnant woman receiving BUP pharmacotherapy was analyzed. BUP was not detected but metabolite concentrations were NBUP-Gluc 46.6, NBUP 15.7 and BUP-Gluc 3.2 ng/g.     

High performance liquid chromatography Ultraviolet method for the determination of fludioxonil fungicide residues: Application on rice grains cultivated in Pakistan

An analytical method was developed and validated for the determination of fludioxonil in rice samples. Rice samples for the study were collected from different regions of Pakistan. The method was based on safe and cost-effective extraction of fludioxonil from rice grains using acetone and methanol (1:1), efficient clean-up through homogenous mixture of acidic aluminium (12 g) and activated charcoal (1 g) followed by liquid chromatographic determination with UV detection. Quantification was performed on Prospher Star C18 (5 µm, 25 × 0.46 cm) column maintaining the temperature 40 °C and detector wavelength 212 nm using mobile phase 50:50 v/v methanol-water (pH 3.3) employing flow rate 1.0 mL min^?1 and 20 µL injection volume. The method showed linearity (0.01–16 mg^?1) with correlation coefficient greater than 0.998. The proposed method was precisely validated for rice sample of all regions, showing recoveries higher than 98%. Rice samples collected from Badin, Multan, Hyderabad, Lahore, Jahania and Sarghoda was found to have fludioxonil residues 0.046, 0.045, 0.043, 0.040, 0.024 and 0.016 mg Kg^?1 respectively, all below the maximum residual limit (MRL) level i.e. 0.05 mg Kg^?1 whereas samples collected from Khanewal and Gularchi showed fludioxonil residue above MRL i.e. 0.065 and 0.058 mg Kg^?1 respectively. However, fludioxonil residues was not detected in rice sample collected from city Makhdumpur.