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

Author(s):  
Tao Lin ◽  
Xinglian Chen ◽  
Li Wang ◽  
Haixian Fang ◽  
Maoxuan Li ◽  
...  

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.

2019 ◽  
Vol 78 ◽  
pp. 02005
Author(s):  
Shaodong Zeng ◽  
jianzhi Ye ◽  
Ling Lin ◽  
wuhai Chen ◽  
Chunliang Yang

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.


Toxins ◽  
2019 ◽  
Vol 11 (2) ◽  
pp. 87 ◽  
Author(s):  
Wenbo Guo ◽  
Kai Fan ◽  
Dongxia Nie ◽  
Jiajia Meng ◽  
Qingwen Huang ◽  
...  

A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six Alternaria toxins. After validation by determining the linearity (R2 > 0.99), recovery (77.8–101.6%), sensitivity (limit of detection in the range of 0.03–0.21 μg kg−1, and limit of quantification in the range of 0.09–0.48 μg kg−1), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of Alternaria toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with Alternaria toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10–1.64 μg kg−1, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the Alternaria toxins contamination in grapes in China.


2020 ◽  
Vol 16 (6) ◽  
pp. 690-697
Author(s):  
Yuedong Yang ◽  
Hao Zhi ◽  
Baofei Yan ◽  
Yi Tian ◽  
Jianping Shen ◽  
...  

Background: The simultaneous determination of multiple components in a sample is an important factor in the quality control of traditional Chinese medicines and can give an indication of potential clinical applications. Introduction: A rapid and sensitive method has been introduced for the simultaneous quantitative analysis of eight bioactive flavonoid constituents from Scutellariae Radix using ultra-high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry. Methods: The separation was performed on a Waters Acquity UPLC C18 column (2.1 mm×100 mm, 1.7 μm), under optimized mass spectrometry conditions, with a flow rate of 0.3 mL/min. The column temperature was maintained at 35°C and the injection volume was 3 μL. Results: The method showed a good linear relationship of each component; all R2 values were above 0.9990 in the experiment. The RSDs of the precision test, repeatability test, stability test and recovery test were all not more than 2.86 %. We found that the total percentage amounts of the eight flavonoids were 22.19%, 18.63% and 10.86% in Raw Scutellariae Radix (RSR), Wine Scutellaria Radix (WSR) and Scutellaria Radix Charcoal (SRC) respectively. Conclusion: The method was successfully applied to the simultaneous determination of the eight bioactive flavonoids of Raw Scutellariae Radix, Wine Scutellaria Radix and Scutellaria Radix Charcoal.


Sign in / Sign up

Export Citation Format

Share Document