scholarly journals A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues

Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 274
Author(s):  
Qiuhong Yang ◽  
Xiaohui Ai ◽  
Jing Dong ◽  
Yongtao Liu ◽  
Shun Zhou ◽  
...  
Keyword(s):  
High Performance ◽  
Procambarus Clarkii ◽  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Experimental Conditions ◽  
Neutral Alumina ◽  
Relative Standard ◽  
Primary Secondary Amine

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues.

Simultaneous Determination of Phenolic Acids, Anthraquinones, and Flavonoids in the Aerial Part and the Fruit of Xanthium Sibiricum by LC- ESI- QTRAP-MS/MS

2019 ◽  
Vol 15 (5) ◽  
pp. 542-553
Author(s):  
Hui Zhao ◽  
Hao Cai ◽  
Juan-Xiu Liu ◽  
Sheng-Nan Wang ◽  
Xun-Hong Liu ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Phenolic Acids ◽  
High Performance ◽  
Aerial Part ◽  
Multiple Reaction Monitoring ◽  
Principal Component ◽  
Negative Ion ◽  
Xanthium Sibiricum ◽  
Relative Standard

Background: Xanthium sibiricum is a well-known traditional Chinese medicine (TCM) that has been commonly used to treat rhinitis and related nasal diseases. The aim of this study was to develop a comprehensive analytical method based on high-performance liquid chromatographyelectrospray ionization coupled with triple quadrupole-linear ion trap mass spectrometry (LC-ESIQTRAP- MS/MS) for the simultaneous determination of phenolic acids, anthraquinones, and flavonoids in the aerial part and fruit of Xanthium sibiricum. Methods: The separation was completed on Agilent ZORBAX SB-C18 column (250 × 4.6 mm, 5μm) using methanol and 0.2% (v/v) aqueous formic acid as the mobile phase. The target components were analyzed in negative ion mode with accurate and sensitive multiple reaction monitoring (MRM) mode. Results: The correlation coefficients of all the calibration curves were higher than 0.9994. Relative standard deviations of intra- and inter-day precisions of the eighteen components were all lower than 2.87% and the recoveries were in the range from 97.73% to 101.82%. The validated method was successfully applied to possess forty Xanthium sibiricum samples (Xanthii Herba, Xanthii Fructus, and processed Xanthii Fructus) collected from different places in P. R. China. Furthermore, principal component analysis (PCA) was performed to evaluate and classify the samples according to the contents of the eighteen bioactive components. Conclusion: All the results demonstrated that the developed method was useful and could be applied for the overall assessment of the quality of Xanthii Herba and Xanthii Fructus.

Rapid determination of patulin in medicinal hawthorn fruits by HPLC-MS/MS

2012 ◽  
Vol 5 (1) ◽  
pp. 31-36 ◽  
Author(s):  
L. Xiang ◽  
Y. Gao ◽  
D. Liu ◽  
M. Yang
Keyword(s):  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Negative Ion ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Hawthorn Fruit ◽  
Negative Ion Mode

An HPLC-tandem mass spectrometry method was developed for the determination of patulin (PAT) in dried medicinal hawthorn fruit, a well-known traditional medicine in China. Liquid-liquid extraction was applied in the sample preparation. Multiple reaction monitoring was performed at m/z 153/109 for PAT and m/z 317/273 for internal standard zearalenone in the negative ion mode with electrospray ionisation source. Good linearity was achieved when spiked PAT concentrations were in the range of 10-500 μg/kg, with coefficient being 0.9993. The limit of quantitation was 10 μg/kg. The extraction recoveries for the spiked PAT at concentrations of 20, 100 and 400 μg/kg were 64.5%, 64.6% and 63.9%, respectively, with relative standard deviations of 1.25%, 2.82% and 2.61%. The intra-day and inter-day precision were in the range of 2.2-9.6% and 5.9-6.4%. This rapid, sensitive and reliable method was applied in 25 batches of medicinal hawthorn fruit, in which PAT was detected in 8 batches, including those that were baked or charred.

Rapid determination of fosetyl-aluminium in commercial pesticide formulations by high-performance liquid chromatography

2014 ◽  
Vol 68 (6) ◽  
Author(s):  
Helen Karasali ◽  
Konstantinos Kasiotis ◽  
Kyriaki Machera
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Hplc Method ◽  
Negative Ion ◽  
Rp Hplc ◽  
Relative Standard

AbstractAn isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method with diode array detection (DAD) was developed for the determination of aluminium tris(ethyl phosphonate) (fosetyl-aluminium, fosetyl-Al) in plant-protection products. The method involves extraction of the active ingredient by sonication of the sample with water and direct measurement by RPHPLC. The isocratic RP-HPLC method for the analysis of fosetyl-Al thus developed was then validated for specificity, linearity, precision, and accuracy. The chromatographic peak confirmation was performed by LC-MS using electron spray ionisation in the negative-ion mode. The repeatability of the method, expressed as relative standard deviation (RSD, %), was found to be 0.5 % and the limit of detection was 0.035 mg mL−1. The average recoveries of the three fortification levels varied from 96.7 % to 100.6 % and the RSDs ranged between 2.6 % and 6.3 %. The precision of the method was also considered to be acceptable as the experimental repeatability relative standard deviation (RSDr) was lower than the RSDr, calculated using the Horwitz equation. The method is rapid, simple, accurate, cost-effective, and provides a new and reliable means for the analysis of fosetyl-Al in formulated products.

scholarly journals Rapid Determination of Chloramphenicol in Tilapia by ultra-high performance liquid chromatography-mass spectrometry

2019 ◽  
Vol 78 ◽  
pp. 02005
Author(s):  
Shaodong Zeng ◽  
jianzhi Ye ◽  
Ling Lin ◽  
wuhai Chen ◽  
Chunliang Yang
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Rapid Determination ◽  
Water Solution ◽  
Multiple Reaction Monitoring ◽  
High Sensitivity ◽  
Relative Standard

A rapid method for the determination of residues of chloramphenicol in tilapia by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The samples were extracted with acetonitrile, and separated on a C18 column using methanol-water solution as mobile phase, and then detected under ESI- multiple reaction monitoring mode. The method showed a good linearity for the analysts over the range of 0.1-100μg/L. The detection limits were 0.10μg/kg. The recoveries ranged from 88.6% to 108% at spiked concentrations with the relative standard deviations lower than 5%. The results shows that this method has the advantages of easy to operate, fast to perform, with high sensitivity and accuracy, and it is suitable for detection of residues of chloramphenicol in tilapia.

Simultaneous Determination of Eight New Generation Amide Insecticide Residues in Complex Matrix Agri-food by Multi-walled Carbon Nanotube Cleanup and UPLC-MS/MS

2021 ◽  
Author(s):  
Tao Lin ◽  
Xinglian Chen ◽  
Li Wang ◽  
Haixian Fang ◽  
Maoxuan Li ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Simultaneous Determination ◽  
High Performance ◽  
Rapid Determination ◽  
Complex Matrix ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
The Matrix ◽  
Multi Walled Carbon Nanotubes

Abstract The simultaneous determination method of 8 amide pesticides by multi-walled carbon nanotubes (MWCNs) cleanup, combined with QuEChERS method and ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry has been developed and successfully applied in complex matrix such as green onions, celery, leeks, citrus, lychees, avocado. The matric effect of MWCNs is optimized and compared with QuEChERS materials. The results show that MWCNs can effectively reduce the matrix effect in sample extraction. The mass spectrometry is optimized, through their chemical structure skeletons, the ESI+ and ESI- mode are simultaneously scanned in the method. The coefficient (r) is greater than 0.9990, the limit of quantification ranges from 0.03 to 0.80 μg/kg, the recovery rate ranges from 71.2% to 120%, and the relative standard deviation (RSD) ranges from 3.8% to 9.4%. The method is fast, simple, sensitive, and has good purification effect. It is suitable for the rapid determination of amide pesticides in complex matrix agri-food.

scholarly journals Multiresidue Method for Determination of Algal Toxins in Shellfish: Single-Laboratory Validation and Interlaboratory Study

2005 ◽  
Vol 88 (3) ◽  
pp. 761-772 ◽  
Author(s):  
Paul McNabb ◽  
Andrew I Selwood ◽  
Patrick T Holland ◽  
J Aasen ◽  
T Aune ◽  
...  
Keyword(s):  
Multiple Reaction Monitoring ◽  
Interlaboratory Study ◽  
Negative Ion ◽  
Shellfish Poisoning ◽  
Algal Toxins ◽  
Validation Data ◽  
Phase Gradient ◽  
Relative Standard ◽  
Single Laboratory

Abstract A method that uses liquid chromatography with tandem mass spectrometry (LC/MS/MS) has been developed for the highly sensitive and specific determination of amnesic shellfish poisoning toxins, diarrhetic shellfish poisoning toxins, and other lipophilic algal toxins and metabolites in shellfish. The method was subjected to a full single-laboratory validation and a limited interlaboratory study. Tissue homogenates are blended with methanol-water (9 + 1), and the centrifuged extract is cleaned up with a hexane wash. LC/MS/MS (triple quadrupole) is used for quantitative analysis with reversed-phase gradient elution (acidic buffer), electrospray ionization (positive and negative ion switching), and multiple-reaction monitoring. Ester forms of dinophysis toxins are detected as the parent toxins after hydrolysis of the methanolic extract. The method is quantitative for 6 key toxins when reference standards are available: azaspiracid-1 (AZA1), domoic acid (DA), gymnodimine (GYM), okadaic acid (OA), pectenotoxin-2 (PTX2), and yessotoxin (YTX). Relative response factors are used to estimate the concentrations of other toxins: azaspiracid-2 and -3 (AZA2 and AZA3), dinophysis toxin-1 and -2 (DTX1 and DTX2), other pectenotoxins (PTX1, PTX6, and PTX11), pectenotoxin secoacid metabolites (PTX2-SA and PTX11-SA) and their 7-epimers, spirolides, and homoYTX and YTX metabolites (45-OHYTX and carboxyYTX). Validation data have been gathered for Greenshell mussel, Pacific oyster, cockle, and scallop roe via fortification and natural contamination. For the 6 key toxins at fortification levels of 0.05–0.20 mg/kg, recoveries were 71–99% and single laboratory reproducibilities, relative standard deviations (RSDs), were 10–24%. Limits of detection were <0.02 mg/kg. Extractability data were also obtained for several toxins by using successive extractions of naturally contaminated mussel samples. A preliminary interlaboratory study was conducted with a set of toxin standards and 4 mussel extracts. The data sets from 8 laboratories for the 6 key toxins plus DTX1 and DTX2 gave within-laboratories repeatability (RSDr) of 8–12%, except for PTX-2. Between-laboratories reproducibility (RSDR) values were compared with the Horwitz criterion and ranged from good to adequate for 7 key toxins (HorRat values of 0.8–2.0).

Rapid Determination of Formaldehyde in Dried Bean Milk Cream by HPLC with Pre-Column Derivatization

2012 ◽  
Vol 554-556 ◽  
pp. 1493-1497
Author(s):  
Qi Tong ◽  
Jian Zheng Song ◽  
Qiu Rong Li
Keyword(s):  
High Performance ◽  
Rapid Determination ◽  
Rapid Test ◽  
Chromatography Method ◽  
System A ◽  
Controlling System ◽  
Relative Standard ◽  
Liquid Chromatography Method ◽  
Set Up

A high-performance liquid chromatography method was set up for rapid determination of formaldehyde in dried bean milk cream. This thesis studies the Nash derivatization, derivative solubility, reaction time, amounts of Nash and derivative stability. The derivative is chromatographic separated by Agilent Zorbax Eclipse XDB-C18 column (4.6mm× 250mm, 5μm) and detected by index detector with VWD (412nm). The heater does not need the temperature-controlling system. A mobile phase was composed of acetonitrile and water (50:50, V/V) at a flow rate of 0.8 mL/min. Under the conditions of the above-mentioned test, the developed calibration curves displayed good linearity over a concentration range of 0.00 to 0.80mg/L, with a correlation coefficient exceeding 0.9998. Average spike recovery was found in a range of 88% to 91%, with a relative standard deviation (RSD) between 1.1% and 4.0%.The minimum detection limit of source is 0.013mg/Kg. The method can be used for rapid test on formaldehyde preservative in dried bean milk cream.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

Rapid Determination of Metronidazole and 2-Hydroxymetronidazole in Murine Blood Plasma

2021 ◽  
Author(s):  
Nina Zemanová ◽  
Pavel Anzenbacher ◽  
Tomáš Hudcovic ◽  
Eva Anzenbacherová
Keyword(s):  
Plasma Proteins ◽  
Mobile Phase ◽  
High Performance ◽  
Rapid Determination ◽  
Internal Standard ◽  
Hplc Method ◽  
Primary Metabolite ◽  
Relative Standard ◽  
Protozoan Infections

Abstract Metronidazole is a drug used to treat bacterial and protozoan infections. Nowadays, it is one of the most frequently prescribed drugs worldwide. The main aim of this paper is to present a rapid, reliable and simple high-performance liquid chromatography (HPLC) method to determine metronidazole along with its primary metabolite, 2-hydroxymetronidazole, in plasma or serum using paracetamol as an internal standard. A total of 100% methanol was used to denature plasma proteins. After centrifugation, the supernatant was evaporated under nitrogen flow. The samples were dissolved in the mobile phase and injected into a Li-Chrospher RP-18 column. A total of 10 mmol/L NaH2PO4: acetonitrile (90:10, v/v) solution with a flow rate of 1 mL/min was used as the mobile phase. Metronidazole and 2-hydroxymetronidazole were detected at two different wavelengths at 320 nm and 311 nm, respectively. The method is characterized by high precision (relative standard deviation % &lt; 6). The method was used for the determination of metronidazole and 2-hydroxymetronidazole in murine blood using small amounts of plasma (≤100 μL).

scholarly journals A Rapid Determination and Quantification of Three Biologically Active Polyisoprenylated Benzophenones using Liquid Chromatography-Tandem Mass Spectrometry (MRM) Method in Five Garcinia species from Cameroon

2017 ◽  
Vol 12 (12) ◽  
pp. 1934578X1701201
Author(s):  
Bernadette Messi Biloa ◽  
Raimana Ho ◽  
Guillaume Marti ◽  
Alain Meli Lannang ◽  
Jean-Luc Wolfender ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Biologically Active ◽  
Ionization Mass ◽  
Relative Standard

Following investigation of Garcinia genus, a sensitive, rapid and simple reversed-phase high performance liquid chromatography-electrospray ionization mass spectrometry method has been developed for the identification and quantification of three polyisoprenylated benzophenones, garcinol (1), isogarcinol (2) and 7- epi-clusianone (3), in the extracts of five Garcinia species from Cameroon. The separation of those compounds was achieved on a RP-18 column using a solvent system consisting of a mixture of acetonitrile-water-formic acid as a mobile phase in a gradient elution mode. The identification of the three compounds was determined on a triple quadripole mass spectrometer with ESI interface operating in the negative mode. A multiple reaction monitoring (MRM) method was developed for the quantification of these polyisoprenylated benzophenones in the extracts of the Garcinia species. The method was validated through intra- and inter-day precision, with the relative standard deviation (RSD) less than 6%, limits of detection (LOD) and limits of quantification (LOQ) <1 ng. Overall recoveries ranged from 94% to 104%, with RSDs ranging from 0.8% to 4.5%. The results indicated that the fruits of G. preussii and the roots of G. brevipedicellata are good source of garcinol (1) and isogarcinol (2) respectively.

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