A Validated LC-MS/MS Method for the Quantification of Trigonelline in Marketed Dietary Supplements

2020 ◽  
Vol 16 (5) ◽  
pp. 687-695 ◽  
Author(s):  
Gullapalli Kowmudi ◽  
Krishnaveni Nagappan ◽  
Karthika Anoop ◽  
Mukkamala Sailaja ◽  
Narenderan S. T.
Keyword(s):  
Dietary Supplements ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ionization Source ◽  
Fenugreek Seeds ◽  
Trigonella Foenum Graecum ◽  
Positive Mode ◽  
Trigonella Foenum Graecum L

Background: Fenugreek seeds are employed in many traditional systems as an antibacterial, antidiabetic agent, gastric stimulant, and also for anti-invasive activity. Therefore, it is a suitable bioactive marker to establish the quality of crude drug and its formulations. Methods: A rapid, simple and sensitive LC-MS/MS analytical method was developed and validated for the determination of trigonelline extracted from Trigonella foenum-graecum (L.) (Fenugreek) and marketed dietary supplements using Etofylline as an internal standard. The objective of the present study is to quantify Trigonelline extracted from Trigonella foenum graecum L. (fenugreek) and marketed dietary supplements. Chromatographic separation was achieved on a Zorbax C18 column (50mm x 4.6mm i.d, 5μ particle size). The samples were eluted using 0.1% Formic acid in water: Methanol (20:80%v/v) at a flow rate of 0.5ml/min with a runtime of 5 min. The eluents were monitored using a tandem mass spectrometer equipped with an electro spray ionization source in positive mode. Results: The analysis was performed in multiple reaction monitoring (MRM) mode by quantifying the ion transitions from m/z 138.0→92.5 (Trigonelline) and m/z 225.0→180.90 (IS). The developed method was linear over the concentration range 5-50 ng/mL. The LOD and LOQ were found to be 1.0 ng/mL and 10.0 ng/mL, respectively. The correlation coefficient (r2) was found to be ≥0.998 for Trigonelline. Conclusion: The proposed validated LC-MS/MS method offers a sensitive quantification of trigonelline in Trigonella foenum graecum L. (fenugreek) and marketed dietary supplements containing fenugreek seeds.

scholarly journals Pharmacokinetic Comparison of Isoalantolactone and Alantolactone in Rats after Administration Separately by Optimization of an UPLC-MS2Method

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Renjie Xu ◽  
Mengyue Wang ◽  
Ying Peng ◽  
Xiaobo Li
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Sprague Dawley ◽  
Ionization Source ◽  
Fragment Ions ◽  
Sprague Dawley Rats ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Ion

Isoalantolactone and alantolactone are two major active ingredients that are present in many medicinal plants. In this study, a sensitive and rapid ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for determination of the two compounds in rat plasma, separately. In this method, an electrospray ionization source was applied and operated in positive ion mode; multiple reaction monitoring (MRM) was selected for quantification using target fragment ions 233.2→187.1 for isoalantolactone (alantolactone) and 245.1→189.1 for internal standard (IS). Retention time of the lactones and IS was within 3.0 min. Further calibration suggested a linear regression can be calculated within 2.5–500 ng/mL for isoalantolactone and 4–500 ng/mL for alantolactone. This method was used to compare the pharmacokinetic characteristics of isoalantolactone and alantolactone at a single dose of 5 mg/kg into male Sprague-Dawley rats by intravenous administration separately. The levels oft1/2, Kel, CL,Cmax, and AUC were significantly increased in the alantolactone group compared to isoalantolactone. These results suggested that isoalantolactone was distributed and eliminated more rapidly than alantolactone in rats when administered, respectively.

scholarly journals Development of a rapid UPLC-MS/MS method for the determination of toddalolactone in mouse blood and its application in pharmacokinetics

2021 ◽  
Author(s):  
Jing Zhou ◽  
Hongzhe Wang ◽  
Caiyun Miao ◽  
Yunxi Yao ◽  
Jianshe Ma
Keyword(s):  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Absolute Bioavailability ◽  
Quantitative Detection ◽  
Ionization Source ◽  
Mouse Blood ◽  
The Matrix ◽  
Product Ions

AbstractA rapid and simple UPLC-MS/MS method was developed to determine toddalolactone in mouse blood and applied to measure the pharmacokinetics of toddalolactone in mice. Blood samples were first preprocessed by ethyl acetate liquid-liquid extraction. Oxypeucedanin hydrate (internal standard, IS) and toddalolactone were gradient eluted from a UPLC BEH C18 column using a mobile phase consisting of acetonitrile and water (0.1% formic acid). Using electrospray ionization (ESI) as the ionization source, multiple reaction monitoring was used to detect the precursor and product ions of m/z 309.2 and 205.2, respectively, for toddalolactone and of m/z 305.1 and 203.0 for IS, respectively, for quantitative detection. A calibration curve was run over the concentration range of 5–4,000 ng/mL (r > 0.995). The matrix effects ranged from 93.5 to 98.4%, and the recovery was higher than 77.3%. The precision was less than 13%, and the accuracy ranged from 90.9 to 108.4%. The developed UPLC-MS/MS method was successfully used for measuring the pharmacokinetics of toddalolactone in mice after oral (20 mg/kg) and intravenous administration (5 mg/kg), and the absolute bioavailability of toddalolactone was 22.4%.

SENSITIVE BIO ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF VENETOCLAX IN HUMAN PLASMA BY LC-ESI-MS/MS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (06) ◽  
pp. 32-38
Author(s):  
H. Potluri ◽  
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Liquid Liquid Extraction ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Development And Validation

A specific and sensitive method of liquid chromatography–tandem mass spectrometry was demonstrated for the experimental determination of venetoclax in human plasma utilising venetoclax-D8 as an internal standard. The column Xbridge C18, 50 × 4.6mm, 5 µm was used for attaining chromatographic separation by utilising 10mM ammonium formate and methanol as isocratic mobile phase in the composition ratio of 20:80 (V/V). The flow-rate selected was 0.7ml/min. Venetoclax and venetoclax-D8 are identified in multiple reaction monitoring (MRM) positive mode with proton adducts at m/z 869.53 →553.21 and m/z 877.14 → 553.23, respectively. For the successful extraction of drug as well as internal standard, liquid-liquid extraction technique was efficiently utilised. The developed technique was established in a linear concentration range of 5.0-5000.0 pg/ml along with correlation coefficient (r2) of 0.9994. Intra and inter-day precisions were found to be 0.7 to 1.90% and 0.7 to 2.0 % for venetoclax and venetoclax-D8, respectively. Accuracy was found to be within 98.6 to 101.99% and 99.17 to 101.14 % for venetoclax and venetoclax-D8, respectively. It was observed that throughout the bench top studies, post-operative stability studies and freeze-thawing cycles, venetoclax retained stability.

scholarly journals Simultaneous determination of sibutramine and its derivatives in weight loss dietary supplements by LC-MS/MS

2020 ◽  
Vol 3 (2) ◽  
pp. 104-114
Author(s):  
Mai Hoa Duong Thi ◽  
Ngoc Mai Pham Thi ◽  
Khanh Cao Cong ◽  
Hong Ngoc Nguyen Thi ◽  
Thanh Hoa Mac Thi ◽  
...  
Keyword(s):  
Weight Loss ◽  
Dietary Supplements ◽  
Ammonium Acetate ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Formic Acid Solution ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode

The liquid chromatography tandem mass spectrometry method (LC-MS/MS) was used to determine the content of sibutramine (SB), N-desmethyl sibutramine (DSB) and N-didesmethyl sibutramine (DDSB) illegaly mixed in weight loss dietary supplements. Sibutramine and its derivatives were extracted by methanol; impurities in the extract were removed by graphitized carbon black (GCB) adsorbent. The chromatographic separation of analytes took place on C18 column (100 mm x 2.1 mm, 3.5 µm) with a gradient mobile phase of acetonitrile and 2 mM ammonium acetate in 0.1% formic acid solution. Multiple reaction monitoring (MRM) in the positive mode was used to detect and quantify SB, DSB and DDSB at m/z 279.9/124.8; 266.0/124.8 and 252.1/125.0, respectively. The method was validated following the AOAC requirements for specificity, repeatability and recovery. Calibration curves lineared from 0.002 to 0.1 µg/mL for SB, DSB and DDSB. The method was successfully applied to determine the content of SB, DSB and DDSB in weight loss dietary supplements that were randomly collected from phamacies in Hanoi of three formulations of hard capsule, soft capsule and teabag. The results shown that six samples had SB and DSB with the content in the range of 0.817 - 31.7 mg/g.

scholarly journals Sensitive Quantification of Liensinine Alkaloid Using a HPLC-MS/MS Method and Its Application in Microvolume Rat Plasma

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Fen Wei ◽  
Xilan Gou ◽  
Xiao Xu ◽  
Sicen Wang ◽  
Tao Bao
Keyword(s):  
Quality Control ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
In Vivo Studies ◽  
Coefficient Of Determination ◽  
Ionization Source ◽  
Limit Of Quantification ◽  
Positive Mode

Liensinine, an important alkaloid in lotus seed, exhibits multiple functions such as anti-AIDS, anticancer, antidepressant, and antihypertensive properties. In this study, a highly sensitive HPLC-MS/MS method was developed and validated for the quantification of liensinine in microvolume rat plasma as low as 45 μL. Chromatographic separation was carried out using a reverse-phase Gemini-C18 column (100 mm × 3 mm i.d. × 5 μm), and mass selective detection using multiple reaction monitoring was attained using an electrospray ionization source, which operated in the positive mode. Dauricine was used as the internal standard. The precursor-to-product ion transition m/z 611.15 > 206.10 was selected for the detection of liensinine; m/z 625.25 > 206.10 was used for the detection of dauricine. The developed method is linear over the concentration range of 0.05–1000 ng/mL with an excellent coefficient of determination (R2 = 0.991). The recoveries ranged from 92.57% to 95.88% at three quality control levels. Intraday and interday precision and accuracy are less than 12.2% and 6.59%, respectively. The lower limit of quantification (LLOQ) is 0.05 ng/mL. The matrix effect was insignificant and acceptable. The validated method was successfully applied to the pharmacokinetic study of liensinine in rats. This method can be used for in vivo studies as well as quality control of traditional Chinese medicines and herbal tea containing liensinine alkaloid.

scholarly journals Enantioseparation and Determination of Penconazole in Rat Plasma by Chiral LC-MS/MS: Application to a Stereoselective Toxicokinetic Study

Molecules ◽  
2020 ◽  
Vol 25 (13) ◽  
pp. 2964
Author(s):  
Siman Ma ◽  
Jia Lun ◽  
Yanru Liu ◽  
Zhen Jiang ◽  
Xingjie Guo
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Rat Plasma ◽  
Male Rats ◽  
Ionization Source ◽  
Established Method ◽  
Relative Standard

In this study, a specific and sensitive method of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the determination of penconazole enantiomers in rat plasma. The enantioseparation was achieved on a Chiralpak IC column by using acetonitrile/water (80:20, v/v) as the mobile phase. Penconazole enantiomers and internal standard l-lansoprazole (IS) were detected in multiple reaction monitoring (MRM) mode with positive electrospray ionization source. The method was validated over the concentration range of 2.5–250.0 ng mL−1 for penconazole enantiomers. Good linearity was obtained for both enantiomers with correlation coefficients (R) greater than 0.995. The relative error was well within the admissible range of −1.1–3.2%, and relative standard deviation was less than 6.0%. After validation, the established method was successfully applied to a stereoselective toxicokinetic study in female and male rats after oral administration of 50 mg kg−1 racemic penconazole. This is the first experiment regarding the stereospecific toxicokinetic study of penconazole and the bioanalytical approach for its quantitation in vivo.

scholarly journals Simultaneous Determination of Reserpine, Rescinnamine, and Yohimbine in Human Plasma by Ultraperformance Liquid Chromatography Tandem Mass Spectrometry

2013 ◽  
Vol 2013 ◽  
pp. 1-11 ◽  
Author(s):  
Muzaffar Iqbal ◽  
Aftab Alam ◽  
Tanveer A. Wani ◽  
Nasr Y. Khalil
Keyword(s):  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Analytical Response ◽  
Positive Mode ◽  
One Step ◽  
Electrospray Interface

A sensitive and selective UPLC-MS/MS method was developed and validated for the determination of three indolic alkaloids (reserpine, rescinnamine, and yohimbine) in human plasma using papaverine as internal standard (IS). After a one step protein precipitation with acetonitrile, separation was carried out using C18 column (50 × 2.1 mm, i.d. 1.7 μm) and mobile phase consisting of acetonitrile : water : formic acid (60 : 40 : 0.1%, v/v/v) pumped at a flow rate of 0.2 mL/min. The mass spectrometric determination was carried out using an electrospray interface operated in the positive mode with multiple reaction monitoring (MRM) mode. The precursor to product ion transitions ofm/z609.32 > 195.01,m/z635.34 > 221.03,m/z355.19 > 144, andm/z340.15 > 202.02 were selected for the quantification of reserpine, rescinnamine, yohimbine, and IS, respectively. The analytical response was found to be linear in the range of 0.36–400, 0.27–300, and 0.23–250 ng/mL with lower limit of quantification of 0.36, 0.27, and 0.23 ng/mL for reserpine, rescinnamine, and yohimbine, respectively. Validation was made following official guidelines. The proposed method enabled reproducible results and hence could be reliable for pharmacokinetic and toxicological analysis.

scholarly journals Eco-Friendly UPLC–MS/MS Method for Determination of a Fostamatinib Metabolite, Tamatinib, in Plasma: Pharmacokinetic Application in Rats

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4663
Author(s):  
Essam Ezzeldin ◽  
Muzaffar Iqbal ◽  
Yousif A. Asiri ◽  
Ahmed Y. A. Sayed ◽  
Rashad Alsalahi
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Liquid Liquid Extraction ◽  
Highly Sensitive ◽  
Multiple Reaction Monitoring Mode ◽  
Positive Mode ◽  
Syk Inhibitor

Fostamatinib is a prodrug of the active metabolite tamatinib, which is a spleen tyrosine kinase (Syk) inhibitor used in the treatment of primary chronic adult immune thrombocytopenia and rheumatoid arthritis. A highly sensitive, rapid, reliable, and green method was developed and validated using ultra-performance liquid chromatography and tandem mass spectrometry (UPLC–MS/MS) for quantification of tamatinib in rat plasma. Ibrutinib was used as internal standard and liquid–liquid extraction was applied using tert-butyl methyl ether. The analyte was separated on an AcquityTM CSH C18 (2.1 mm × 100 mm, 1.7 µm) column using mobile phase consisting of 10 mM ammonium acetate and acetonitrile (10:90) and the flow rate was 0.25 mL/min. Electrospray ionization (ESI) was carried out in positive mode. Quantitation of tamatinib and the IS was performed using multiple reaction monitoring mode with precursor-to-product transitions of m/z 471.1 > 122.0 and m/z 441.1 > 84.0, respectively. The calibration range was 0.1–1000.0 ng/mL and the linearity of the method was ≥0.997. The developed method greenness was investigated. All principal parameters for the method, including linearity, accuracy, precision, recovery, and stability, were within acceptable ranges. Tamatinib pharmacokinetic study in rats was successfully carried out using the developed method.

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