分散固相萃取-液相色谱-串联质谱法测定淡水鱼中柱孢藻毒素、节球藻毒素和微囊藻毒素
|
摘要
建立了同时检测淡水鱼中柱孢藻毒素、节球藻毒素、微囊藻毒素-RR、微囊藻毒素-YR及微囊藻毒素-LR的分散固相萃取-液相色谱-串联质谱方法。样品粉碎后,用乙腈-水-甲酸(89∶10∶1, v/v/v)提取目标物,C_(18)分散固相萃取柱净化,Agilent ZORBAX Eclipse XDB C_(18)色谱柱分离,乙腈和水梯度洗脱,在多反应监测(MRM)模式下进行定性分析,基质匹配标准曲线外标法定量。考察了提取溶剂及吸附剂种类对提取效率和净化效果的影响,并优化了液相色谱-串联质谱条件。该法在各自范围内具有良好线性关系,相关系数(R~2)≥0.995 4;检出限为5～10μg/kg,定量限为15～40μg/kg;样品的加标回收率为62.3%～101.2%。该方法前处理方法简单快速,灵敏高效,适用于淡水鱼中柱孢藻毒素、节球藻毒素和微囊藻毒素的有效检测。
A method was developed for the determination of cylindrospermopsin(CYN), nodularin(NOD), microcystin-RR(MC-RR), microcystin-YR(MC-YR) and microcystin-LR(MC-LR) in freshwater fish by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry(DSPE-LC-MS/MS). The analytes were extracted from fish tissues with acetonitrile-water-formic acid(89∶10∶1, v/v/v), and purified by DSPE using C_(18) as the adsorbent. The separation of analytes was performed on an Agilent ZORBAX Eclipse XDB C_(18) column with the gradient elution of acetonitrile and water as mobile phases. Qualitative analysis was performed using the multiple reaction monitoring(MRM) mode. The analytes were quantified by matrix-matched external standard curves. The chromatographic and MS parameters were optimized. Major factors affecting the extraction and cleanup efficiencies including the type of extraction solvent and cleanup sorbent were investigated. The linear correlation coefficients(R~2) of the five target compounds were no less than 0.995 4. The limits of detection(LODs, S/N=3) and limits of quantification(LOQs, S/N=10) of the five target compounds were 5-10 μg/kg and 15-40 μg/kg, respectively. The spiked recoveries of the five target compounds ranged from 62.3% to 101.2%. The developed method is simple, rapid, accurate, sensitive, and is suitable for the determination of cylindrospermopsin, nodularin and microcystins in freshwater fish.
A method was developed for the determination of cylindrospermopsin(CYN), nodularin(NOD), microcystin-RR(MC-RR), microcystin-YR(MC-YR) and microcystin-LR(MC-LR) in freshwater fish by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry(DSPE-LC-MS/MS). The analytes were extracted from fish tissues with acetonitrile-water-formic acid(89∶10∶1, v/v/v), and purified by DSPE using C_(18) as the adsorbent. The separation of analytes was performed on an Agilent ZORBAX Eclipse XDB C_(18) column with the gradient elution of acetonitrile and water as mobile phases. Qualitative analysis was performed using the multiple reaction monitoring(MRM) mode. The analytes were quantified by matrix-matched external standard curves. The chromatographic and MS parameters were optimized. Major factors affecting the extraction and cleanup efficiencies including the type of extraction solvent and cleanup sorbent were investigated. The linear correlation coefficients(R~2) of the five target compounds were no less than 0.995 4. The limits of detection(LODs, S/N=3) and limits of quantification(LOQs, S/N=10) of the five target compounds were 5-10 μg/kg and 15-40 μg/kg, respectively. The spiked recoveries of the five target compounds ranged from 62.3% to 101.2%. The developed method is simple, rapid, accurate, sensitive, and is suitable for the determination of cylindrospermopsin, nodularin and microcystins in freshwater fish.
引文
[1] Corbel S,Mougin C,Bouaicha N.Chemosphere,2014,96(2):1
[2] Otten T G,Xu H,Qin B,et al.Environ Sci Technol,2012,46(6):3480
[3] Karlsson K,Sipia V,Krause E,et al.Environ Toxicol,2003,18(5):284
[4] Zheng J,Zhang W,Chi H Q,et al.Strait Journal of Preventive Medicine,2016,22(3):60 郑竟,张薇,池慧钦,等.海峡预防医学杂志,2016,22(3):60
[5] Lei L M,Peng L,Huang X H,et al.Environ Model Assess,2014,186(5):3079
[6] Hawkins P R,Runnegar M T C,Jackson A R B,et al.Environ Microbiol,1985,50(5):1292
[7] Fang X J,Gao H Y,Chen H J,et al.Journal of Chinese Institute of Food Science and Technology,2011,11(2):209 房祥军,郜海燕,陈杭君,等.中国食品学报,2011,11(2):209
[8] Xu H,Jiang M,Wang J.Journal of Instrumental Analysis,2015,34(9):1072 许慧,江敏,王婧.分析测试学报,2015,34(9):1072
[9] Shen F,Xu Y J,Jiang S,et al.Journal of Analytical Science,2018,34(1):95 沈斐,许燕娟,姜晟,等.分析科学学报,2018,34(1):95
[10] Zhang X Y,Cai X X,Zhang X Y,et al.Chinese Journal of Chromatography,2017,35(12):1286 张秀尧,蔡欣欣,张晓艺,等.色谱,2017,35(12):1286
[11] Pekar H,Westerberg E,Bruno O,et al.J Chromatogr A,2016,1429:265
[12] Cui Y W,Li S Y,Yang X Q,et al.Food Anal Methods,2018,11(6):1748
[13] Li S,Cui Y,Wang Y,et al.Food Chem,2018,269:89
[14] Greer B,Maul R,Campbell K,et al.Anal Bioanal Chem,2017,409(16):4057
[15] Vudathala D,Smith S,Khoo L,et al.Toxicon,2017,138:82
[16] Li S Y,Wang Y,Wang D N,et al.Chinese Journal of Chromatography,2017,35(8):794 李诗言,王扬,王鼎南,等.色谱,2017,35(8):794
[17] Anastassiades M,Lehotay S J,Stajnbaher D.J AOAC Int,2003,86 (2):41
[18] Li J,Sun L,Jin M N,et al.Chinese Journal of Chromatography,2019,37(2):177 励炯,孙岚,金朦娜,等.色谱,2019,37(2):177
[19] Liu T F,Yang D F,Zhang X M,et al.Chinese Journal of Chromatography,2018,36(10):1028 刘腾飞,杨代凤,章雪明,等.色谱,2018,36(10):1028
[20] Qin L,Dong Y L,Wang G L,et al.Chinese Journal of Chromatography,2018,36(9):880 覃玲,董亚蕾,王钢力,等.色谱,2018,36(9):880
[21] Rodrigues M A,Reis M P,Mateus M C.Toxicon,2013,74:8
[22] Gambaro A,Barbaro E,Zangrando R,et al.Rapid Commun Mass Spectrom,2012,26(12):1497
[23] Kikuchi S,Kubo T,Kaya K.Anal Chim Acta,2007,583(1):124
[24] Guzmán-Guillén R,Moreno I,Ortega A I P,et al.Talanta,2015,131:452
[25] SN/T 4319-201
[26] Moreno I M,Molina R,Jos A,et al.J Chromatogr A,2005,1080(2):199
[27] Geis-Asteggiante L,Lehotay S J,Fortis L L,et al.Anal Bioanal Chem,2011,401(8):2617
[28] Barbieri M V,Postigo C,Guillem-Argiles N,et al.Sci Total Environ,2019,653:958
[29] Li J,Zhang J,Liu H,et al.J Sci Food Agric,2016,96(2):555
[30] Moschou I C,Dasenaki M E,Thomaidis N S.J Chromatogr B,2019,1104:134
[31] Su Y Z,Li F,Qi X,et al.Journal of Analytical Sciences,2015,32(2):203 粟有志,李芳,齐鑫,等.分析科学学报,2015,32(2):203
[32] Yang X T,Tang X Y,Shen X X.Chinese Journal of Analytical Chemistry,2017,45(7):1019 杨小体,汤晓艳,沈习习.分析化学,2017,45(7):1019
[33] Wang R G,Su X O,Wang P L,et al.Chinese Journal of Analytical Chemistry,2017,45(2):231 王瑞国,苏晓鸥,王培龙,等.分析化学,2017,45(2):231
[34] Zhao L,Lucas D,Long D,et al.J Chromatogr A,2018,1549:14
[2] Otten T G,Xu H,Qin B,et al.Environ Sci Technol,2012,46(6):3480
[3] Karlsson K,Sipia V,Krause E,et al.Environ Toxicol,2003,18(5):284
[4] Zheng J,Zhang W,Chi H Q,et al.Strait Journal of Preventive Medicine,2016,22(3):60 郑竟,张薇,池慧钦,等.海峡预防医学杂志,2016,22(3):60
[5] Lei L M,Peng L,Huang X H,et al.Environ Model Assess,2014,186(5):3079
[6] Hawkins P R,Runnegar M T C,Jackson A R B,et al.Environ Microbiol,1985,50(5):1292
[7] Fang X J,Gao H Y,Chen H J,et al.Journal of Chinese Institute of Food Science and Technology,2011,11(2):209 房祥军,郜海燕,陈杭君,等.中国食品学报,2011,11(2):209
[8] Xu H,Jiang M,Wang J.Journal of Instrumental Analysis,2015,34(9):1072 许慧,江敏,王婧.分析测试学报,2015,34(9):1072
[9] Shen F,Xu Y J,Jiang S,et al.Journal of Analytical Science,2018,34(1):95 沈斐,许燕娟,姜晟,等.分析科学学报,2018,34(1):95
[10] Zhang X Y,Cai X X,Zhang X Y,et al.Chinese Journal of Chromatography,2017,35(12):1286 张秀尧,蔡欣欣,张晓艺,等.色谱,2017,35(12):1286
[11] Pekar H,Westerberg E,Bruno O,et al.J Chromatogr A,2016,1429:265
[12] Cui Y W,Li S Y,Yang X Q,et al.Food Anal Methods,2018,11(6):1748
[13] Li S,Cui Y,Wang Y,et al.Food Chem,2018,269:89
[14] Greer B,Maul R,Campbell K,et al.Anal Bioanal Chem,2017,409(16):4057
[15] Vudathala D,Smith S,Khoo L,et al.Toxicon,2017,138:82
[16] Li S Y,Wang Y,Wang D N,et al.Chinese Journal of Chromatography,2017,35(8):794 李诗言,王扬,王鼎南,等.色谱,2017,35(8):794
[17] Anastassiades M,Lehotay S J,Stajnbaher D.J AOAC Int,2003,86 (2):41
[18] Li J,Sun L,Jin M N,et al.Chinese Journal of Chromatography,2019,37(2):177 励炯,孙岚,金朦娜,等.色谱,2019,37(2):177
[19] Liu T F,Yang D F,Zhang X M,et al.Chinese Journal of Chromatography,2018,36(10):1028 刘腾飞,杨代凤,章雪明,等.色谱,2018,36(10):1028
[20] Qin L,Dong Y L,Wang G L,et al.Chinese Journal of Chromatography,2018,36(9):880 覃玲,董亚蕾,王钢力,等.色谱,2018,36(9):880
[21] Rodrigues M A,Reis M P,Mateus M C.Toxicon,2013,74:8
[22] Gambaro A,Barbaro E,Zangrando R,et al.Rapid Commun Mass Spectrom,2012,26(12):1497
[23] Kikuchi S,Kubo T,Kaya K.Anal Chim Acta,2007,583(1):124
[24] Guzmán-Guillén R,Moreno I,Ortega A I P,et al.Talanta,2015,131:452
[25] SN/T 4319-201
[26] Moreno I M,Molina R,Jos A,et al.J Chromatogr A,2005,1080(2):199
[27] Geis-Asteggiante L,Lehotay S J,Fortis L L,et al.Anal Bioanal Chem,2011,401(8):2617
[28] Barbieri M V,Postigo C,Guillem-Argiles N,et al.Sci Total Environ,2019,653:958
[29] Li J,Zhang J,Liu H,et al.J Sci Food Agric,2016,96(2):555
[30] Moschou I C,Dasenaki M E,Thomaidis N S.J Chromatogr B,2019,1104:134
[31] Su Y Z,Li F,Qi X,et al.Journal of Analytical Sciences,2015,32(2):203 粟有志,李芳,齐鑫,等.分析科学学报,2015,32(2):203
[32] Yang X T,Tang X Y,Shen X X.Chinese Journal of Analytical Chemistry,2017,45(7):1019 杨小体,汤晓艳,沈习习.分析化学,2017,45(7):1019
[33] Wang R G,Su X O,Wang P L,et al.Chinese Journal of Analytical Chemistry,2017,45(2):231 王瑞国,苏晓鸥,王培龙,等.分析化学,2017,45(2):231
[34] Zhao L,Lucas D,Long D,et al.J Chromatogr A,2018,1549:14