scholarly journals A Convenient and Sensitive LC-MS/MS Method for Simultaneous Determination of Carbadox- and Olaquindox-Related Residues in Swine Muscle and Liver Tissues

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
Heying Zhang ◽  
Wei Qu ◽  
Yanfei Tao ◽  
Dongmei Chen ◽  
Shuyu Xie ◽  
...  
Keyword(s):  
Carboxylic Acid ◽  
Simultaneous Determination ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Free Form ◽  
Anion Exchange Column ◽  
Tissue Samples ◽  
Metaphosphoric Acid ◽  
Liver Tissues

This paper presents a convenient and sensitive LC-MS/MS method for the simultaneous determination of carbadox and olaquindox residues, including desoxyolaquindox (DOLQ), desoxycarbadox (DCBX), quinoxaline-2-carboxylic acid (QCA), 3-methyl-quinoxaline-2-carboxylic acid (MQCA), and the glycine conjugates of QCA and MQCA (namely, QCA-glycine and MQCA-glycine, resp.) in swine muscle and liver tissues. Tissue samples were extracted with 2% metaphosphoric acid in 20% methanol and cleaned up by solid-phase extraction (SPE) on a mixed-mode anion-exchange column (Oasis MAX). Analysis was performed on a C18 column by detection with mass spectrometry in the multiple reaction monitoring (MRM) mode. The limits of detection (LODs) of the six analytes were determined to be 0.01 μg·kg−1 to 0.25 μg·kg−1, and the limits of quantification (LOQs) were 0.02 μg·kg−1 to 0.5 μg·kg−1. The total recoveries of the six analytes in all tissues were higher than 79.1% with the RSD% less than 9.2%. The developed method can determine the real residue level of QCA and MQCA, whether they are present in free form or as glycine conjugates in tissues, together with the carcinogenic desoxy metabolites DCBX and DOLQ with high recovery. Therefore, this method was suitable for routine analysis of residue control programmes and the residue depletion study of CBX and OLQ on swine.

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.

scholarly journals Simultaneous Determination of 34 Amino Acids in Tumor Tissues from Colorectal Cancer Patients Based on the Targeted UHPLC-MS/MS Method

2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Yang Yang ◽  
Feng Zhang ◽  
Shouhong Gao ◽  
Zhipeng Wang ◽  
Mingming Li ◽  
...  
Keyword(s):  
Colorectal Cancer ◽  
Amino Acids ◽  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Tissue Homogenate ◽  
Ionization Source ◽  
Tissue Samples

A targeted ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was established and validated for the simultaneous determination of 34 amino acids in tissue samples from colorectal cancer (CRC) patients. The chromatographic separation was achieved on an Agilent ZORBAX SB-C18 column (3.0 × 150 mm, 5 μm) with a binary gradient elution system (A, 0.02% heptafluorobutyric acid and 0.2% formic acid in water, v/v; B, methanol). The run time was 10 min. The multiple reaction monitoring mode was chosen with an electrospray ionization source operating in the positive ionization mode for data acquisition. The linear correlation coefficients were >0.99 for all the analytes in their corresponding calibration ranges. The sample was pretreated based on tissue homogenate and protein precipitation with a 100 mg aliquot sample. The average recovery and matrix effect for 34 amino acids and 3 internal standards were 39.00%∼146.95% and 49.45%∼173.63%, respectively. The intra- and interday accuracy for all the analytes ranged from −13.52% to 14.21% (RSD ≤8.57%) and from −14.52% to 12.59% (RSD ≤10.31%), respectively. Deviations of stability under different conditions were within ±15% for all the analytes. This method was applied to simultaneous quantification of 34 amino acids in tissue samples from 94 CRC patients.

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.

Simultaneous determination of phenytoin and dextromethorphan in urine by solid-phase extraction and HPLC-DAD

2005 ◽  
Vol 28 (11) ◽  
pp. 1157-1162 ◽  
Author(s):  
Natale Alfredo Santagati ◽  
Roberto Gotti ◽  
Giuseppe Ronsisvalle
Keyword(s):  
Solid Phase Extraction ◽  
Simultaneous Determination ◽  
Solid Phase ◽  
Phase Extraction
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