Simultaneous Determination of Eight Potential Q-Markers in Zishen Tongguan Capsules Based on UHPLC-MS/MS

2020 ◽  
Vol 17 (1) ◽  
pp. 47-56
Author(s):  
Shun Liu ◽  
Xun Wang ◽  
Kaiping Zou ◽  
Wei Liu ◽  
Cunyu Li ◽  
...  
Keyword(s):  
Quality Control ◽  
Chinese Medicine ◽  
Simultaneous Determination ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Quality Markers ◽  
High Repeatability ◽  
Comprehensive Study

Background: Zishen Tongguan (ZSTG) capsules were prepared at the Affiliated Hospital of Nanjing University of Chinese Medicine and have been proven to be clinically effective for treating pyelonephritis and benign prostatic hyperplasia. However, the quality standards are not ideal; a comprehensive study of the “quality markers” (Q-markers), the chemicals inherent in traditional Chinese medicine and its preparations, has not been carried out. Experimental Methods: In this paper, a sensitive and specific ultra-high-performance liquid chromatographictandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of eight potential Q-markers of ZSTG, including timosaponin A3, berberine, jatrorrhizine, phellodendrine, palmatine, mangiferin, neomangiferin, and timosaponin BII. A Kromasil 100-3.5 C18 column was used with a mobile phase of 0.2% formic acid with acetonitrile, and gradient elution at a flow rate of 0.2 mL/min was achieved in 13 minutes and used for separation. Detection was performed in positive/negative mode with multiple reaction monitoring (MRM). Results: The analytical method was validated in terms of the sensitivity, linearity, accuracy, precision, repeatability, stability and recovery. The method established here was successfully applied to study the potential Q-markers in 8 batches of commercial samples, which demonstrated its use in improving the quality control of ZSTG. Conclusion: The developed method had high repeatability and accuracy and was suitable for the simultaneous analysis of multiple Q-markers, which may provide a new basis for the comprehensive assessment and overall quality control of ZSTG.

A UPLC-MS/MS Assay for Simultaneous Determination of Two Antipsychotics and Two Antidepressants in Human Plasma and Its Application in Clinic

2020 ◽  
Vol 21 (1) ◽  
pp. 60-69
Author(s):  
Houli Li ◽  
Xiaoliang Cheng ◽  
Di Zhang ◽  
Maoyi Wang ◽  
Weihua Dong ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Medication Compliance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Individual Therapy ◽  
Therapeutic Drug ◽  
Ionization Source

Background: Antidepressants and antipsychotics are widely prescribed drugs for the treatment of mental diseases. Therapeutic drug monitoring (TDM) is recommended for patients taking these drugs to ensure pharmaceutical efficacy, medication compliance and prevent toxicity. Objective: An ultra-high performance liquid chromatography/tandem-mass spectrometry (UPLC-MS/ MS) method was developed for simultaneous determination of two Antidepressants-Fluoxetine (FLU) and Escitalopram (ESC), and two antipsychotics-risperidone (RIS) and aripiprazole (ARI), in human plasma. Methods: The sample was processed by simple protein precipitation and the targeted analytes were separated on a C18 column by gradient elution with a mobile phase containing 0.1% formic acid (v/v) and acetonitrile. All the analytes were qualitative and quantitative measured by electrospray ionization source with Multiple Reaction Monitoring (MRM) in positive ion mode. A total of 56 plasma samples were obtained from out- or in-patients who were taking the cited four drugs for further analysis. Results: The calibration curves for FLU, ESC, RIS and ARI were linear in the range of 45-1800, 4-320, 2-200 and 50-1800 ng/mL, respectively. The entire analytical time for the analytes was 7.0 min for each run and the extraction efficiency was more than 90%. The sample was stable within various storage conditions. The trough concentrations in patients were measured with the validated method. Conclusions: The developed method was successfully used for simultaneous determination of FLU, ESC, RIS and ARI in the plasma of the patients, which provides effective technical support for routine TDM of these four drugs and is of great clinic value for individual therapy.

Environmentally Evaluated New HPLC/UV Method for the Simultaneous Determination of Acesulfame-K, Butylated Hydroxytoluene, and Aspartame and Its Degradant in Chewing Gum

2019 ◽  
Vol 102 (6) ◽  
pp. 1892-1900
Author(s):  
Nada S. Zamzam ◽  
Mona H. Abdel Rahman ◽  
Maha F. Abdel Ghani
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Low Cost ◽  
Food Additives ◽  
Gradient Elution ◽  
Butylated Hydroxytoluene ◽  
Chewing Gum ◽  
Adverse Health Effects ◽  
Chewing Gums

Background: Acesulfame-K (ACE), butylated hydroxytoluene (BHT), and aspartame (ASP) are a common combination of food additives added to chewing gums. The abuse of these additives results in severe adverse health effects; however, they are still extensively used owing to their high performance and low cost. Objective: The development and optimization of a simple, cheap, sensitive, and eco-friendly HPLC/UV method for the simultaneous determination of ASP, ACE, and BHT along with aspartame degradation product phenylalanine (PHEN) in chewing gum. Methods: The method was optimized using a 5 μm C18 column and an eluent consisting of methanol and 0.1 M phosphate buffer (pH 5.0) according to a suitable gradient elution program. Simple sample preparation, consisting of dilution, homogenization, and sonication followed by centrifugation and filtration, was optimized and used for the extraction of chewing gum. The greenness of the method was evaluated. Results: The proposed method exhibited excellent linearity (R2 > 0.9996), low LOQ (0.08–0.95 μg/mL), and recoveries between 85.3 and 98.83% with relative SD (RSD) ≤ 2.7%. High resolution was obtained with <25 min run times with excellent precision (RSD: 0.28–1.33%). This method was successfully applied for the simultaneous determination of ACE, ASP, and BHT in commercial chewing gum; PHEN was not detected. Furthermore, our method is considered to be environmentally acceptable. Conclusions: The results demonstrate that the developed method can be used to detect ACE, BHT, ASP, and PHEN in chewing gum. Highlights: A new sensitive, green HPLC/UV method is developed to be used as a minimal-cost routine analysis procedure for commercial chewing gum.

Environmentally Evaluated New HPLC/UV Method for the Simultaneous Determination of Acesulfame-K, Butylated Hydroxytoluene, and Aspartame and Its Degradant in Chewing Gum

2019 ◽  
Vol 102 (6) ◽  
pp. 1892-1900
Author(s):  
Nada S Zamzam ◽  
Mona H Abdel Rahman ◽  
Maha F Abdel Ghani
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Low Cost ◽  
Food Additives ◽  
Gradient Elution ◽  
Butylated Hydroxytoluene ◽  
Chewing Gum ◽  
Adverse Health Effects ◽  
Chewing Gums

Abstract Background: Acesulfame-K (ACE), butylated hydroxytoluene (BHT), and aspartame (ASP) are a common combination of food additives added to chewing gums. The abuse of these additives results in severe adverse health effects; however, they are still extensively used owing to their high performance and low cost. Objective: The development and optimization of a simple, cheap, sensitive, and eco-friendly HPLC/UV method for the simultaneous determination of ASP, ACE, and BHT along with aspartame degradation product phenylalanine (PHEN) in chewing gum. Methods: The method was optimized using a 5 μm C18 column and an eluent consisting of methanol and 0.1 M phosphate buffer (pH 5.0) according to a suitable gradient elution program. Simple sample preparation, consisting of dilution, homogenization, and sonication followed by centrifugation and filtration, was optimized and used for the extraction of chewing gum. The greenness of the method was evaluated. Results: The proposed method exhibited excellent linearity (R2 &gt; 0.9996), low LOQ (0.08–0.95 μg/mL), and recoveries between 85.3 and 98.83% with relative SD (RSD) ≤ 2.7%. High resolution was obtained with &lt;25 min run times with excellent precision (RSD: 0.28–1.33%). This method was successfully applied for the simultaneous determination of ACE, ASP, and BHT in commercial chewing gum; PHEN was not detected. Furthermore, our method is considered to be environmentally acceptable. Conclusions: The results demonstrate that the developed method can be used to detect ACE, BHT, ASP, and PHEN in chewing gum. Highlights: A new sensitive, green HPLC/UV method is developed to be used as a minimal-cost routine analysis procedure for commercial chewing gum.

scholarly journals Simultaneous Determination of Four Major Constituents of Semen Vaccariae Using HPLC-DAD

2012 ◽  
Vol 7 (9) ◽  
pp. 1934578X1200700 ◽  
Author(s):  
Haijiang Zhang ◽  
Wei Yao ◽  
Yunyun Chen ◽  
Peipei He ◽  
Yao Chen ◽  
...  
Keyword(s):  
Quality Control ◽  
Quantitative Analysis ◽  
Simultaneous Determination ◽  
Chromatographic Separation ◽  
Gradient Elution ◽  
Hplc Method ◽  
Frying Temperature ◽  
Simultaneous Quantification ◽  
Frying Process

A simple and reliable HPLC method was developed and validated for the simultaneous quantification of four major constituents in Semen Vaccariae. The chromatographic separation was performed on an Agilent Zorbax SB-C18 column with gradient elution using methanol and water. The calibration curves showed good linearity of R2 > 0.9999 with LOQs (S/N = 10) of 0.20–1.16 μg/mL. The precision was evaluated by intra- and inter-day assays and R.S.D. values were less than 2.09%. The recovery rates were between 97.0% and 105.0%. The developed method was applied to the quantitative analysis of Semen Vaccariae and its stir-fried products. During the stir-frying process, vaccarin degraded and yielded isovitexin-2″- O-arabinoside. The preferable stir-frying temperature is around 120°C. The developed HPLC method can be applied to the quality control of crude and stir-fried Semen Vaccariae.

scholarly journals Simultaneous Determination of Eight Synthetic Permitted and Five Commonly Encountered Nonpermitted Food Colors in Various Food Matrixes by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (5) ◽  
pp. 1503-1514 ◽  
Author(s):  
Sumita Dixit ◽  
Subhash K Khanna ◽  
Mukul Das
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Food Category ◽  
Food Commodities ◽  
Food Colors

Abstract A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 -Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.99740.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two-to seven-fold higher than those prescribed.

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 A Simple High-Performance Liquid Chromatography Method for Simultaneous Determination of Three Triazole Antifungals in Human Plasma

2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Internal Standard ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.

scholarly journals Determination of Polypeptide Antibiotic Residues in Food of Animal Origin by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3261
Author(s):  
Tomasz Bladek ◽  
Iwona Szymanek-Bany ◽  
Andrzej Posyniak
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Animal Origin ◽  
Antibiotic Residues ◽  
Triple Quadrupole Mass Spectrometer ◽  
Limit Of Quantification ◽  
Food Of Animal Origin ◽  
Polypeptide Antibiotic

A novel UHPLC-MS/MS method for the determination of polypeptide antibiotic residues in animal muscle, milk, and eggs was developed and validated. Bacitracin A, colistin A, colistin B, polymyxin B1, and polymyxin B2 were extracted from the samples with a mixture of acetonitrile/water/ammonia solution 25%, 80/10/10 (v/v/v), and put through further evaporation, reconstitution, and filtration steps. The chromatographic separation was performed on a C18 column in gradient elution mode. Mass spectral acquisitions were performed in selective multiple reaction monitoring mode by a triple quadrupole mass spectrometer. The method was validated according to the criteria of Commission Decision 2002/657/EC. The method quantifies polypeptides in a linear range from 10 to 1000 μg kg−1, where the lowest concentration on the calibration curve refers to the limit of quantification (LOQ). The recoveries ranged from 70 to 99%, the repeatability was below 13%, and within-laboratory reproducibility was lower than 15%. The decision limit (CCα) and detection capability (CCβ) values were calculated, and ruggedness and stability studies were performed, to fulfill the criteria for confirmatory methods. Moreover, the developed method may also be used for screening purposes by its labor efficiency.

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