Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS

In this study, an external standard quantitative method for the determination of ethyl carbamate content in cheese by GC-MS/MS was established, the pretreatment conditions of the sample were optimized, and the methodology of the detection method was investigated. The results showed that the optimal...

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Main Author: LIANG Jianying, TANG Shuo, LIU Lijun, XIE Ruilong, GAO Yujie, HU Xue, LI Cuizhi, LV Zhiyong
Format: Article
Language:English
Published: Editorial Department of China Brewing 2024-04-01
Series:Zhongguo niangzao
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Online Access:https://manu61.magtech.com.cn/zgnz/fileup/0254-5071/PDF/0254-5071-2024-43-4-253.pdf
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author LIANG Jianying, TANG Shuo, LIU Lijun, XIE Ruilong, GAO Yujie, HU Xue, LI Cuizhi, LV Zhiyong
author_facet LIANG Jianying, TANG Shuo, LIU Lijun, XIE Ruilong, GAO Yujie, HU Xue, LI Cuizhi, LV Zhiyong
author_sort LIANG Jianying, TANG Shuo, LIU Lijun, XIE Ruilong, GAO Yujie, HU Xue, LI Cuizhi, LV Zhiyong
collection DOAJ
description In this study, an external standard quantitative method for the determination of ethyl carbamate content in cheese by GC-MS/MS was established, the pretreatment conditions of the sample were optimized, and the methodology of the detection method was investigated. The results showed that the optimal pretreatment conditions were as follows: 2 ml of deionized water was added to the sample for mixing, 1 ml of acetonitrile was added for extraction, the sample was centrifuged at 0 ℃ and 6 000 r/min for 8 min, the supernatant was cleaned-up by an alkaline diatomaceous earth solid-phase extraction cartridge (2 g/10 ml), n-hexane drenching, eluted with 20 ml dichloromethane, nitrogen blown against the eluent to about 0.5 ml, and then the supernatant was set volume with methanol for GC-MS/MS detection and quantified by external standard method. The method was linear in the mass concentration range of 5-200 ng/ml with the correlation coefficient R<sup>2</sup>&gt;0.99. The limit of quantification (LOQ) was 0.01 mg/kg, the limit of detection (LOD) was 0.005 mg/kg, the recovery rates ranged from 69.1% to 90.7% in the experinents of standard recovery rates of high, middle and low addition levels, and the relative standard deviations (RSDs) of the results of the precision tests ranged from 4.2% to 11.1%. The method was easy to operate, accurate and suitable for the determination of ethyl carbamate content in cheese.
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publishDate 2024-04-01
publisher Editorial Department of China Brewing
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spelling doaj-art-2adc35ef080a4809825a09c2cd62091f2025-08-20T02:45:56ZengEditorial Department of China BrewingZhongguo niangzao0254-50712024-04-0143425325710.11882/j.issn.0254-5071.2024.04.038Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MSLIANG Jianying, TANG Shuo, LIU Lijun, XIE Ruilong, GAO Yujie, HU Xue, LI Cuizhi, LV Zhiyong01. Inner Mongolia Yili Industrial Group Co., Ltd., Hohhot 010110, China; ;2. National Key Laboratory for Market Supervision (Milk and Milk Products Testing and Monitoring Technology), Shanghai 200127, ChinaIn this study, an external standard quantitative method for the determination of ethyl carbamate content in cheese by GC-MS/MS was established, the pretreatment conditions of the sample were optimized, and the methodology of the detection method was investigated. The results showed that the optimal pretreatment conditions were as follows: 2 ml of deionized water was added to the sample for mixing, 1 ml of acetonitrile was added for extraction, the sample was centrifuged at 0 ℃ and 6 000 r/min for 8 min, the supernatant was cleaned-up by an alkaline diatomaceous earth solid-phase extraction cartridge (2 g/10 ml), n-hexane drenching, eluted with 20 ml dichloromethane, nitrogen blown against the eluent to about 0.5 ml, and then the supernatant was set volume with methanol for GC-MS/MS detection and quantified by external standard method. The method was linear in the mass concentration range of 5-200 ng/ml with the correlation coefficient R<sup>2</sup>&gt;0.99. The limit of quantification (LOQ) was 0.01 mg/kg, the limit of detection (LOD) was 0.005 mg/kg, the recovery rates ranged from 69.1% to 90.7% in the experinents of standard recovery rates of high, middle and low addition levels, and the relative standard deviations (RSDs) of the results of the precision tests ranged from 4.2% to 11.1%. The method was easy to operate, accurate and suitable for the determination of ethyl carbamate content in cheese.https://manu61.magtech.com.cn/zgnz/fileup/0254-5071/PDF/0254-5071-2024-43-4-253.pdfcheese|ethyl carbamate|gc-ms/ms|pretreatment conditions optimization
spellingShingle LIANG Jianying, TANG Shuo, LIU Lijun, XIE Ruilong, GAO Yujie, HU Xue, LI Cuizhi, LV Zhiyong
Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS
Zhongguo niangzao
cheese|ethyl carbamate|gc-ms/ms|pretreatment conditions optimization
title Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS
title_full Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS
title_fullStr Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS
title_full_unstemmed Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS
title_short Optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by GC-MS/MS
title_sort optimization of pretreatment conditions for determination of ethyl carbamate content in cheese by gc ms ms
topic cheese|ethyl carbamate|gc-ms/ms|pretreatment conditions optimization
url https://manu61.magtech.com.cn/zgnz/fileup/0254-5071/PDF/0254-5071-2024-43-4-253.pdf
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