scholarly journals Simultaneous Determination of Methamphetamine and Its Isomer N-Isopropylbenzylamine in Forensic Samples by Using a Modified LC-ESI-MS/MS Method

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Yangxu Luo ◽  
Juan Du ◽  
Huadi Xiao ◽  
Ling Zheng ◽  
Xuncai Chen ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Acetate Solution ◽  
Accurate Identification ◽  
Esi Ms ◽  
Target Analytes ◽  
Relative Standard ◽  
Forensic Samples

Accurate identification and quantification of methamphetamine (MA) and its related substances are essential for the investigation and fair trial of drug offenses. In this study, a modified LC-ESI-MS/MS method for the simultaneous determination of MA and its isomer N-isopropylbenzylamine (N-IBA) in forensic samples was developed and validated. Optimum chromatographic separation of the target analytes was achieved on an Agilent Poroshell 120 SB-C18 column ( 4.6 × 100  mm, 2.7 μm) at 40°C with isocratic elution at the flow rate of 0.40 mL/min. The mobile phase was acetonitrile and 20 mM ammonium acetate solution containing 0.1% formic acid (80 : 20, v / v ). Positive ESI-MS/MS detection was performed in multiple reaction monitoring (MRM) mode to identify and quantify the target analytes. Method validation showed excellent linearity in the range of 0.51 ng/mL~51 ng/mL for MA and N-IBA. The low limit of detection (LLOD) and low limit of quantification (LLOQ) reached 0.1 ng/mL and 0.3 ng/mL for both analytes. The method showed a satisfactory accuracy with an inter- and intraday-relative error (RE) <20%, and a precision of inter- and intraday relative standard deviation (RSD) less than 15%. The validated method was successfully applied in real forensic samples and resulted in the detection of MA and N-IBA in 8 suspected samples in drug cases that only deemed MA positive using our previous routine screening procedure, which avoided the misidentification of N-IBA as MA.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals UPLC–MS/MS simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, MDMA, and MDA in hair

2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Ammonium Hydroxide ◽  
Ultra Performance Liquid Chromatography ◽  
Acetate Solution ◽  
Hair Samples ◽  
Relative Standard

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

Simultaneous determination of five pesticides residues in Anoectochilus roxburghii by HPLC-MS/MS method

2020 ◽  
Vol 20 (5) ◽  
pp. 345-349
Author(s):  
Liqun WU ◽  
◽  
Mingke LUO ◽  
Wensheng HE ◽  
Wenting CHEN
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Acetonitrile Solution ◽  
Ionization Source ◽  
Thiophanate Methyl ◽  
Pesticides Residues ◽  
Relative Standard ◽  
Anoectochilus Roxburghii

Objective： To establish a HPLC-MS/MS method for simultaneous determination of five pesticides residues including tebuconazole，metalaxyl-M，thiophanate-methyl，oxytetracycline and abamectin in Anoectochilus roxburghii.Methods： The samples were extracted by acetonitrile solution and purified by QuEChERS method.Separation was performed on Agilent Eclipse Plus C18 column（50 mm×2.1 mm，1.8 μm） with the mobile phase consisting of 0.1% formic acid（A） and acetonitrile（B） by gradient elution（0-1.0 min，90% A；1.0-3.0 min，90%-70% A;3.0-5.0 min，70%-30% A;5.0-8.0 min，30%-10% A;8.0-14.0 min，10% A;14.0-15.0 min，10%-90% A;15.0-17.0 min，90% A）.Detection was performed on a triple quadrupole tandem mass spectrometry with electrospray ionization source operating in positive ion mode under multiple reaction monitoring（MRM） mode.Results： The calibration curves of five pesticides showed good linearity coefficients（r>0.99）.The average recoveries ranged from 72.7% to 94.9%（n=6），and the relative standard derivations（RSDs） were within 1.8%-10.3%（n=6）.The detection limits of tebuconazole，metalaxyl-M，thiophanate-methyl，oxytetracycline and abamectin were 0.6，0.2，0.3，0.2，5.0 μg/kg，and the quantitation limits of 5 pesticides were 2.0，0.5，1.0，0.6 and 10.0 μg/kg respectively.Conclusion： The established method was proved to be sensitive，simple and reliable，and could be applied for the determination of these five pesticides in Anoectochilus roxburghii and quality control in the planting process.

scholarly journals Determination of Pharmaceutical Residues by UPLC-MS/MS Method: Validation and Application on Surface Water and Hospital Wastewater

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Bui Van Hoi ◽  
Cam-Tu Vu ◽  
Lan-Anh Phung-Thi ◽  
Thao Thi Nguyen ◽  
Phuong Thanh Nguyen ◽  
...  
Keyword(s):  
Surface Water ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Hospital Wastewater ◽  
Esi Ms ◽  
Pharmaceutical Residues ◽  
Detection Frequency

In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005–0.015 µg L−1 and 0.014–0.123 µg L−1, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.

Simultaneous Determination of 12 Bioactive Constituents in Bupi Yiqi No. 1 Recipe by Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry

2020 ◽  
Vol 103 (1) ◽  
pp. 117-123
Author(s):  
Qingling Xie ◽  
Bin Li ◽  
Feibing Huang ◽  
Mengru Cao ◽  
Hanwen Yuan ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Cancer Recurrence ◽  
Correlation Coefficients ◽  
Bioactive Constituents ◽  
Column Temperature ◽  
Ginsenoside Re ◽  
Esi Ms ◽  
Stability And Accuracy

Abstract Background: Bupi Yiqi No. 1 Recipe (BPYQ), a traditional Chinese medicine formula, has been widely used as a treatment of multidrug resistance during chemotherapy in colorectal cancer and for the prevention of gastrointestinal cancer recurrence for decades. Objective: In this study, a rapid, reliable, and accurate ultrahigh-performance LC (UHPLC) coupled with electrospray ionization (ESI)–tandem MS (MS/MS) method was developed for the simultaneous determination of 12 major bioactive components, including protocatechuic acid, astilbin, rutin, calycosin-7-O-β-D-glucoside, ginsenoside Re, ononin, isoliquiritigenin, calycosin, apigenin, ginsenoside Rb1, formononetin, and glycyrrhizic acid in BPYQ. Methods: The chromatographic separation of the analytes was achieved on a Poroshell 120 SB-Aq column (50 × 2.1 mm, 1.7 µm) with a mobile phase of acetonitrile and 0.1% (v/v) formic acid aqueous solution. The flow rate and column temperature were set at 0.4 mL/min and 30°C, respectively. Mass spectrometric detection of the analyses was performed on multiple reaction monitoring mode in positive and negative ESI mode. Results: The established UHPLC–ESI–MS/MS method was validated in terms of the linearity, precision, repeatability, stability, and accuracy. All calibration curves of the 12 compounds showed good linearity, with correlation coefficients (r) greater than 0.9980 within the test ranges. The LODs and LOQs for the 12 compounds were in the ranges of 0.08–1.32 and 0.27–5.28 ng/mL, respectively. The average recoveries of all the standard compounds were between 98.4 and 102.9%, and their relative SD values ranged from 1.24 to 3.78%. Conclusions: The proposed method can provide a meaningful basis for the QC of BPYQ. Highlights: The established UHPLC-ESI-MS/MS method was demonstrated to be a powerful tool for quantifying the 12 compounds in BPYQ.

scholarly journals Simultaneous Determination of 17 Sulfonamides and the Potentiators Ormetoprim and Trimethoprim in Salmon Muscle by Liquid Chromatography with Tandem Mass Spectrometry Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 343-348 ◽  
Author(s):  
Ross A Potter ◽  
B Garth Burns ◽  
Jeffrey M van de Riet ◽  
David H North ◽  
Rozina Darvesh
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Fish Tissue ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Relative Standard

Abstract A simple, robust method using liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the simultaneous determination of 17 sulfonamides sulfanilamide (SNL), sulfacetamide (SAA), sulfaguanidine (SGD), sulfapyridine (SPY), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethoxazole (SOZ), sulfamoxole (SXL), sulfisoxazole (SXZ), sulfamethizole (SML), sulfamethazine (SMZ), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfachloropyridazine (SCP), sulfaquinoxaline (SQX), and sulfadimethoxine (SDM) and 2 potentiators ormetoprim (OMP) and trimethoprim (TMP) in fish tissue has been developed. The analytes were extracted from homogenized fish tissue with wateracetonitrile (50 + 50). The extract was clarified by centrifugation and a portion defatted with hexane. The analytes were partitioned into chloroform and evaporated to dryness. The redissolved residue was applied to a C18 reversed-phase column with a wateracetonitrile (0.1% acetic acid) gradient. All of the compounds were completely separated and detected in &lt;10 min at 30°C using LC/MS/MS. Standard curves were linear over the range of 0.02 to 5 ng injected. The limit of detection varied from 0.1 ng/g for SMZ and OMP to 0.9 ng/g for SXL and SOZ. Recoveries varied from 100% for SDM, SOZ, and SQX and 85% for SMR, OMP, and TMP to approximately 30% for SAA. Relative standard deviations for repeat analysis varied from 4% for SMZ and SCP to 23% for SAA.

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.

Simultaneous determination of aflatoxin B1, aflatoxin B2, mycophenolic acid and sterigmatocystin in grape pomace by UHPLC-MS/MS

2014 ◽  
Vol 7 (2) ◽  
pp. 121-129 ◽  
Author(s):  
L. Luan ◽  
N. Chen ◽  
Z. Han ◽  
X. Liu ◽  
Y. Zheng ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Mycophenolic Acid ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Reversed Phase ◽  
Grape Pomace ◽  
Relative Standard ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Aflatoxin B

A reliable ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of aflatoxin B1, aflatoxin B2, mycophenolic acid and sterigmatocystin in grape pomace. The samples were extracted by acetonitrile aqueous solution and further purified using a solid-phase extraction-based homemade clean-up cartridge. Next, the analytes were separated on a reversed-phase C18 column with a mobile phase consisting of water and acetonitrile. The separated compounds were detected with a tandem quadrupole mass spectrometer operating in positive electro-spray ionisation mode using multiple reaction monitoring. The established method was extensively validated by determining linearity (R2≯0.999), recovery (97.5-102.8%) and precision (relative standard deviation ≤7.0%). This method was then used for the simultaneous determination of the four mycotoxins in grape pomace samples.

Simultaneous Determination of Cationic and Anionic Surfactants in Domestic, Sewage and River Effluent by Diffuse Reflectance -Fourier Transform Infrared Spectroscop ic Analysis

2021 ◽  
Vol 30 (1) ◽  
pp. 32-40 ◽  
Author(s):  
Ramsingh Kurrey ◽  
Kaushlya Thakur ◽  
Swati Chandrawanshi ◽  
Manas Kanti Deb
Keyword(s):  
Fourier Transform ◽  
Standard Deviation ◽  
Simultaneous Determination ◽  
Diffuse Reflectance ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Fourier Transform Infrared ◽  
Domestic Sewage ◽  
Relative Standard

A new, simple, rapid and precise novel hyphenated diffuse reflectance-Fourier transform infrared spectroscopy (DRS-FTIR) technique for the simultaneous determination of the most frequently used cationic surfactants (CS+) i.e. cetyltrimethylammonium bromide (CTAB) and anionic surfactant (AS-) i.e. sodium dodecyl sulphate (SDS) in domestic, sewage and river wastewater samples has been stabilised. CS+ and AS- were analyzed using DRS-FTIR, the most steady and strongest vibrational IR peak at 2917.13 cm-1 for CTAB and 1226.07 for SDS were selected for the simultaneous quantiflcation of CS+ and AS- under the optimized condition such as effect of samples volume and effect of temperature. The limit of detection (LOD) and limit of quantiflcation (LOQ) of the present method were 5 µg/mL and 15 µg/mL, respectively. The absorbance and peak area were determined by the DRS-FTIR method, which shows excellent linearity with a correlation coefflcient value of 0.985 and 0.981 for the concentration range of 10-100 µg/mL. The standard deviation (SD) and relative standard deviation (RSD) for six replicate measurements were found to be 0.052 µg/L and 2.8 %, respectively.

scholarly journals Simultaneous Determination of Aspirin and Rosuvastatin Calcium in Capsules by Using RP-HPLC Coupled with Photo Diode Array Detection

2014 ◽  
Vol 33 ◽  
pp. 218-230
Author(s):  
Ankita Panchal ◽  
Gaurav Sanghvi ◽  
Ashish Vachhani ◽  
Navin Sheth ◽  
Devendra Vaishnav
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Lower Limit ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Rosuvastatin Calcium

A simple, sensitive, specific, and cost effective method for simultaneous determination of Aspirin and Rosuvastatin calcium was developed and validated in single dosage formulation. The sample solution of ASP and RSTC was prepared using methanol as a solvent. Separation of ASP and RSTC was achieved with a mobile phase consisting of 20 mM KH2PO4 : Methanol (30:70 v/v) at a flow rate of 1.0 ml/min. Separations were performed on Merck hibar 250-4.6 RP18 (5 µm) column (150 mm X 3.0 mm), using a Shimadzu Prominence HPLC system equipped with a Shimadzu SPD-20A detector, Rhenodyne 7725i injector with 20 μL loop, LC-20 AD pump, CBM-20 Alite controller and LC Solution software. Retention times of ASP and RSTC were 3.747 and 5.969 minutes respectively. Absolute recovery of ASP and RSTC was 100.3 and 100.03 % respectively. The lower limit of quantification (LLOQ) of ASP and RSTC was 0.3097 and 0.1063 ppm and lower limit of detection (LLOD) of ASP and RSTC was 0.01535 and 0.01358 ppm respectively. Linearity was established for the range of concentrations 15.00-90.0 μg/ml and 2.0-12.0 μg/ml for ASP and RSTC respectively with the coefficient of determination (R2) of 0.994 and 0.999 for both the compounds. The inter- and intra-day precision in the measurement of ASP quality control (QC) sample 75 μg/ml, were in the range 0.1-0.2 % relative standard deviation (R.S.D.) and 0.2-0.3 % R.S.D., respectively. The inter- and intra-day precision in the measurement of RST quality control (QC) sample 10 μg/ml, were in the range 0.1-0.2 % R.S.D., and 0.0-0.3 % R.S.D., respectively. The developed method would be applicable for routine quality control of ASP And RSTC in bulk as well as in pharmaceutical formulations

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