Synthesis of Stable Isotope Labeled D5-Cyhalothrin, D5-Fenpropathrin and D5-Fenvalerate from Deuterium Phenol

2021 ◽  
Vol 18 ◽  
Author(s):  
Zhongjie Xu ◽  
Shaofei Bai ◽  
Liyan Shen ◽  
Yong Luo ◽  
Zuming Hu
Keyword(s):  
Mass Spectrometry ◽  
Stable Isotope ◽  
1H Nmr ◽  
Internal Standard ◽  
Starting Material ◽  
Synthetic Route ◽  
Isotopic Enrichment ◽  
High Chemical ◽  
Isotope Abundance

: A convenient synthetic route of deuterium-labeled D5-cyhalothrin, D5-fenpropathrin, and D5-fenvalerate is described with 98.7%, 98.5%, and 98.3% isotopic enrichment and high chemical purities using D6-phenol as labeled starting material. These structures and isotope-abundance were confirmed by 1H NMR and mass spectrometry. The prepared D5-cyhalothrin, D5-fenpropathrin, and D5-fenvalerate can be used as an internal standard reagent for the determination of residual pyrethroids of food and environment.

scholarly journals Determination of S-Adenosylmethionine and S-Adenosylhomocysteine in Plasma and Cerebrospinal Fluid by Stable-Isotope Dilution Tandem Mass Spectrometry

2000 ◽  
Vol 46 (10) ◽  
pp. 1650-1656 ◽  
Author(s):  
Eduard A Struys ◽  
Erwin E W Jansen ◽  
Kees de Meer ◽  
Cornelis Jakobs
Keyword(s):  
Mass Spectrometry ◽  
Cerebrospinal Fluid ◽  
Stable Isotope ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Internal Standard ◽  
Tandem Mass ◽  
Analytical Technique

Abstract Background: Available methods for the determination of nanomolar concentrations of S-adenosylmethionine (SAM) and S-adenosylhomocysteine (SAH) in plasma and cerebrospinal fluid (CSF) are time-consuming. We wished to develop a method for their rapid and simultaneous measurement. Methods: We used tandem mass spectrometry (MS/MS) for the simultaneous determination of SAM and SAH, with stable-isotope-labeled internal standards. The 13C5-SAH internal standard was enzymatically prepared using SAH-hydrolase and [13C5]adenosine. The method comprises a weak anion-exchange solid-phase extraction procedure serving as clean-up step for the deproteinized plasma and CSF samples. After clean-up, samples were injected on a C18 HPLC column, which was connected directly to the tandem mass spectrometer, operating in MS/MS mode. Results: In plasma samples, the intraassay CVs for SAM and SAH were 4.2% and 4.0%, respectively, and the interassay CVs were 7.6% and 5.9%, respectively. In CSF, the intraassay CVs for SAM and SAH were 6.8% and 6.9%, respectively, and the interassay CVs were 4.2% and 5.5%, respectively. Mean recovery of SAM and SAH for both matrices at two concentrations was 93%. Detection limits for SAM and SAH in samples were 7.5 and 2.5 nmol/L, respectively. Concentrations of SAM and SAH in plasma from healthy subjects were within the previously reported ranges. In 10 CSF samples, the mean concentrations (range) were 248 (137–385) nmol/L for SAM and 11.3 (8.9–14.1) nmol/L for SAH. Conclusions: SAM and SAH can be analyzed by MS/MS, taking optimal advantage of the speed and high sensitivity and specificity of this relatively new analytical technique.

Measurement of sodium valproate in serum by direct-insertion chemical-ionization/mass spectrometry.

1980 ◽  
Vol 26 (1) ◽  
pp. 147-149
Author(s):  
G M Schier ◽  
I E Gan ◽  
B Halpern ◽  
J Korth
Keyword(s):  
Mass Spectrometry ◽  
Stable Isotope ◽  
Sodium Valproate ◽  
Chromatographic Separation ◽  
Chemical Ionization ◽  
Internal Standard ◽  
Ionization Mass Spectrometry ◽  
Chemical Ionization Mass Spectrometry ◽  
Ionization Mass

Abstract To quantitatively determine sodium valproate, we use a stable isotope-labeled internal standard and chemical-ionization/mass spectrometry, without prior chromatographic separation. The technique is rapid, simple, sensitive, and provides for the routine analysis of 100 microL of serum with good within-day and day-to-day precision. The technique also allows for the simultaneous determination of phenobarbital, mephobarbital, carbamazepine, primidone, and phenytoin.

Measurement of sodium valproate in serum by direct-insertion chemical-ionization/mass spectrometry.

1980 ◽  
Vol 26 (1) ◽  
pp. 147-149 ◽  
Author(s):  
G M Schier ◽  
I E Gan ◽  
B Halpern ◽  
J Korth
Keyword(s):  
Mass Spectrometry ◽  
Stable Isotope ◽  
Sodium Valproate ◽  
Chromatographic Separation ◽  
Chemical Ionization ◽  
Internal Standard ◽  
Ionization Mass Spectrometry ◽  
Chemical Ionization Mass Spectrometry ◽  
Ionization Mass

Abstract To quantitatively determine sodium valproate, we use a stable isotope-labeled internal standard and chemical-ionization/mass spectrometry, without prior chromatographic separation. The technique is rapid, simple, sensitive, and provides for the routine analysis of 100 microL of serum with good within-day and day-to-day precision. The technique also allows for the simultaneous determination of phenobarbital, mephobarbital, carbamazepine, primidone, and phenytoin.

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