Determination of Ethyl Carbamate in Chinese Yellow Rice Wine by Diatomaceous Earth Extraction and GC/MS Method

2015 ◽  
Vol 98 (3) ◽  
pp. 834-838 ◽  
Author(s):  
Pinggu Wu ◽  
Liqun Zhang ◽  
Xianghong Shen ◽  
Liyuan Wang ◽  
Yan Zou ◽  
...  

Abstract A sensitive and rapid analytical method based on alkaline diatomaceous earth extraction followed by GC/MS was developed for the quantitative determination of the toxic contaminant ethyl carbamate (EC) in yellow rice wines. The optimal extraction conditions were investigated. With the application of diatomaceous earth extraction, the damage of organic acids to the capillary column was greatly reduced. By using d5-EC as an internal standard for quantitative analysis of EC, the linearity of the calibration curves was good between 10 and 1000 ng/mL. The LOD and LOQ were 1.7 and 5.0 μg/kg, respectively. The spiked level of EC was 5.0–300 μg/kg, and the average recovery of the spikes was between 78.4 and 98.2%, with an RSD between 4.3 and 8.3%. Upon validation by five laboratories when spiked with 50, 100, and 300 μg/kg, the average respective recoveries were 102.9, 102.2, and 98.7% with a RSD between 0.7 and 8.1%. The validation results demonstrated that the method is fast, simple, selective, and suitable for the determination of EC in yellow rice wines.


2020 ◽  
pp. 13-16
Author(s):  
A. Y. Khrushchev ◽  
E. R. Akmaev ◽  
V. O. Bondarenko ◽  
A. E. Metlin

In this article we proposed a method for quantitative determination of active substance in pharmaceuticals via Raman scattering using potassium ferricyanide as internal standard. We approved this method in ketoprophenum quantitative determination in drug for veterinary use “Ketojekt”. The calculation of metrological requirements of procedures are established proposed method of calibration. Either we demonstrated the focalisation factor of laser beam affects on the method reproducibility. The method provides a precise, rapid, convenient to quantitative analysis that is more effective than the standard HPLC assay.



2020 ◽  
Vol 12 (7) ◽  
pp. 988-995
Author(s):  
Xiaoyan Xiang ◽  
Xianda He ◽  
Wentang Xia ◽  
Jianguo Yin ◽  
Xiaoli Yuan ◽  
...  

Raman spectroscopy with an internal standard and peak height ratio was applied for the quantitative analysis of dichloromethane and titanium tetrachloride.



Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 479
Author(s):  
Shihan Wang ◽  
Yuanshuai Gan ◽  
Hong Kan ◽  
Xinxin Mao ◽  
Yongsheng Wang

As one of the featured products in northeast China, Oviductus Ranae has been widely used as a nutritious food, which contains a variety of bioactive unsaturated fatty acids (UFAs). It is necessary to establish a scientific and reliable determination method of UFA contents in Oviductus Ranae. In this work, six principal UFAs in Oviductus Ranae, namely eicosapentaenoic acid (EPA), linolenic acid (ALA), docosahexaenoic acid (DHA), arachidonic acid (ARA), linoleic acid (LA) and oleic acid (OA), were identified using UPLC-MS/MS. The UFAs identified in Oviductus Ranae were further separated based on the optimized RP-HPLC conditions. Quantitative analysis of multi-components by single-marker (QAMS) method was implemented in content determination of EPA, ALA, DHA, ARA and OA, where LA was used as the internal standard. The experiments based on Taguchi design verified the robustness of the QAMS method on different HPLC instruments and chromatographic columns. The QAMS and external standard method (ESM) were used to calculate the UFA content of 15 batches of Oviductus Ranae samples from different regions. The relative error (r < 0.73%) and cosine coefficient showed that the two methods obtained similar contents, and the method validations met the requirements. The results showed that QAMS can comprehensively and effectively control the quality of UFAs in Oviductus Ranae which provides new ideas and solutions for studying the active components in Oviductus Ranae.



2021 ◽  
Author(s):  
Yiwen Cao ◽  
Shenjie Zhu ◽  
Lin Zhang ◽  
Qun Cui ◽  
Haiyan Wang

Aiming at the difficulty in qualitative and quantitative analysis of trace compositions in food preservative propionic acid, the trace compositions and the key components influencing the total aldehyde content in...



1987 ◽  
Vol 70 (6) ◽  
pp. 1031-1032
Author(s):  
Yuuko S Endoh ◽  
Ryozo Yamaoka ◽  
Nobuo Sasaki

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.



1972 ◽  
Vol 9 (1) ◽  
pp. 36-42 ◽  
Author(s):  
Calvert C. Bristol

X-ray powder diffraction methods, successful in quantitative determination of silicate minerals in fine-grained rocks, have been applied to the determination of calcite, dolomite, and magnesite in greenschist facies meta-volcanic rocks. Internal standard graphs employing two standards (NaCl and Mo) have been determined.Carbonate mineral modes (calcite and dolomite) for 6 greenschist facies meta-volcanic rocks obtained by the X-ray powder method have been compared to normative carbonate mineral contents calculated for the same rocks. This comparison showed a maximum variation of 7.7 wt.% between the X-ray modes and the normative carbonate mineral contents of the rocks. Maximum standard deviation for the X-ray modes of these rocks was equivalent to 4.4 wt.%.



1971 ◽  
Vol 51 (3) ◽  
pp. 447-454 ◽  
Author(s):  
W. COOPER ◽  
M. G. COYLE ◽  
J. A. MILLS

SUMMARY A method is described for estimating oestriol in 2–10 ml samples of human pregnancy peripheral plasma. It incorporates acid hydrolysis, chemical purification, methylation, chromatography on alumina columns, formation of a derivative and quantitative determination by gas chromatography. A radioactive internal standard was added to correct for procedural losses. Plasma oestriol determinations in five normal patients throughout pregnancy and delivery are reported.



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