線上基質去除技術結合液相層析串聯質譜儀檢測雞肉中馬杜拉黴素

On-line matrix elimination technique coupled liquid chromatography tandem mass spectrometry for analysis of maduramicin in chicken meat

張凱鈞(Kai-Chun Chang)

指導教授 ： 鄭建業

中原大學/理學院/化學研究所/碩士(2010年)

https://doi.org/10.6840/cycu201000856

摘要

馬杜拉黴素為離子型抗球蟲藥，添加於飼料中以防治雞隻球蟲症，養雞業者若使用不慎容易造成雞肉中之藥物殘留，故為了防範雞肉食品中馬杜拉黴素的殘留問題，必須建立精確準確及快速有效率的檢驗方法進行檢測，以維護消費者食用安全。本研究以創新的管柱轉換技術進行雞肉樣品萃取液線上基質去除，再結合液相層析電噴灑離子化離子阱串聯質譜儀檢測雞肉中馬杜拉黴素之殘留。離子阱質譜儀的偵測使用正離子多重反應監測模式，定量方法使用後管柱連續注入內標準品的方式，以減少分析樣品與內標準品於不同時間離子化時所產生的誤差，並減低使用昂貴同位素內標準品的需求。標準檢量線之線性範圍在0~1 ng/mL 時R2 為0.999，偵測極限值可達0.08 ng/mL，定量極限值為0.28 ng/mL。以標準品添加測試雞肉樣品中四種濃度(0.5、1.0、5.0與10.0 ng/mL)，得分析之準確度範圍為84~97%。另於同一天內重複測試此四種濃度樣品之相對標準差為3.7~5.0%，而於不同天重複測試此四種濃度樣品之相對標準差為5.8~7.9%。樣品分析一次的時間為10 min。整體而言，所發展之方法具有快速，良好的靈敏度、重複性、再現性及準確度，並成功的應用在雞肉中馬杜拉黴素的殘留分析。

關鍵字

線上基質去除 ； 管柱轉換技術 ； 液相層析電噴灑離子化離子阱質譜儀 ； 馬杜拉黴素

並列摘要

The ionophoric coccidiostats Maduramicin (MAD) are widely used as an additive in chicken feed to prevent coccidiosis. If excessive amount of MAD are added to the chicken feed by the chicken farmer, it may cause the problem of MAD residues in chicken meat. In order to prevent the problem of MAD abused chicken feed, a precise, accurate and rapid analytical method for examining MAD in chicken meat must be developed. The purpose of this study was to develop an on-line matrix elimination technique coupled liquid chromatography-electrospray-ion trap tandem mass spectrometric method for the analysis of maduramicin in chicken meat. Multiple reaction monitoring in a positive ion mode was used for the detection of MAD with the liquid chromatography-electrospray tandem mass spectrometry. The quantification method was by the continuous postcolumn infusion of internal standard. This novel quantitative method can reduce the error produced by the ionization of MAD and internal standard at different time and can reduce the need of isotopic internal standard. The linear concentration range of the calibration curve was from 0~1 ng/mL (R2 = 0.999). The limit of detection (LOD) was 0.08 ng/mL and limit of quantification (LOQ) was 0.28 ng/mL. The spiking experiments at four different concentration levels of MAD, 0.5, 1.0, 5.0, and 10.0 ng/mL, in chicken meat samples were 84~97%. The inter-day and intra-day precision obtained by measuring the 5, 10, 50, and 100 ng/g standard samples were 3.7~5.0% and 5.8~7.9%, respectively. The analysis time for one sample was 10 mimutes. Overall, the developed method exhibited with rapid analysis, good sensitivity, reproducibility, repeatability, and accuracy for the analysis of maduramicin residue in chicken meat.

並列關鍵字

Liquid chromatography - electrospray ion trap tandem mass spectrometry ； Column switching technique ； On-line matrix elimination ； Maduramicin.

參考文獻

2.Sharma N., Bhalla A., Varma S., Jain S. and Singh S., Toxicity of Maduramicin, Emergency medicine journal, 2005, 22, 880-882.

5.Jestoi M., Rokka M. and Peltonen K., An integrated sample preparation to determine coccidiostats and emerging Fusarium-mycotoxins in various poultry tissues with LC-MS/MS; Molecular nutrition & food research, 2007, 51, 625-637.

6.Rajan S., Tsou H., Mowery P. C., Bullock M. W. and Stockton G. W., Natural abundance quantum 13C NMR spectroscopy of Maduramicin a polyether ionophore antibiotic and coccidiostats; The journal of antibiotics, 1984, XXXVII(11), 1495-1500.

7.Duke R., The Komarowski Reaction; Analytical chemistry, 1947, 19, 661.

8.Gliddon M., Wright D., Markantonatos A. and Groth W., Determination of Maduramicin ammonium in poultry feedstuffs by high-performance liquid chromatography; Analyst, 1988, 113, 813-816.