固相萃取-高效液相色谱-二极管阵列检测器法同时测定湖水中10种蓝藻毒素
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摘要
建立了固相萃取-高效液相色谱-二极管阵列检测器法测定湖水中10种蓝藻毒素(MC-RR、MC-YR、MC-Hty R、MC-LR、MC-WR、MC-LA、MC-LY、MC-LW、MC-LF和NOD)的方法。水样经固相萃取净化后,用Waters PAH C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈和含0.05%三氟乙酸为流动相梯度洗脱,流速为0.8 m L/min,柱温为30℃,进样量为20μL,二极管阵列检测器检测范围190~300 nm,检测波长为238 nm。根据保留时间、二极管阵列检测器全扫描光谱和色谱峰纯度分析等进行定性分析。10种蓝藻毒素在0.05~2.00 mg/L浓度范围内线性关系良好,线性系数R为0.9998~0.9999,方法检出限为0.005~0.020μg/L。3个浓度加标水平(0.1、1.0和1.8 mg/L)的回收率为85.1%~105.3%,相对标准偏差为0.8%~9.2%。本方法适用范围广、操作简单、分析速度快、灵敏度高、重现性和回收率好,采用多重定性增强了定性分析的准确性,可用于实际湖水中10种蓝藻毒素的测定。
A method has been developed by solid phase extraction-high performance liquid chromatography coupled with photodiode array detector for simultaneous determination of 10 kinds of cyanotoxins in lake water,including microcystin-RR( MC-RR),MC-YR,MC-Hty R,MC-LR,MC-WR,MC-LA,MC-LY,MC-LW,MC-LF and nodularin( NOD). The samples were enriched and purified by a HLB solid phase extraction column. The separation was performed on a Waters C18 column( 250 mm×4.6 mm,5 μm) with the gradient elution of acetonitrile and water containing 0.05% trifluoroacetic acid. The flow rate of the mobile phase was 0.8 m L/min. The column temperature was 30℃ and the injection volume was 20 μL. The photodiode array detector was scanned from 190 nm to 300 nm and the detection wavelength was 238 nm. Multiple qualitative analyses were completed according to retention time,full scanning spectrum of photodiode array detector and purity analysis of chromatographic peak. Good linearity was observed in the cyanotoxin concentration range of0.05 mg/L-2. 0 mg/L with correlation coefficients( R) from 0. 9998 to 0. 9999. The limits of detection for10 cyanotoxins were in the range of 0. 005 μg/L-0. 020 μg/L. The recoveries were in the range of 85. 1%-105.3% at the three spiked levels of 0.1 mg/L,1.0 mg/L and 1.8 mg/L with the relative standard deviations( RSD) of 0.8%-9.2%. The method was characterized by wide applicability,convenient operation,quick analytical rate,high sensitivity,good accuracy and high recovery. The qualitative accuracy was improved by using multiple qualitative analyses. This method was successfully applied to determination of 10 kinds of cyanotoxins in lake water.
A method has been developed by solid phase extraction-high performance liquid chromatography coupled with photodiode array detector for simultaneous determination of 10 kinds of cyanotoxins in lake water,including microcystin-RR( MC-RR),MC-YR,MC-Hty R,MC-LR,MC-WR,MC-LA,MC-LY,MC-LW,MC-LF and nodularin( NOD). The samples were enriched and purified by a HLB solid phase extraction column. The separation was performed on a Waters C18 column( 250 mm×4.6 mm,5 μm) with the gradient elution of acetonitrile and water containing 0.05% trifluoroacetic acid. The flow rate of the mobile phase was 0.8 m L/min. The column temperature was 30℃ and the injection volume was 20 μL. The photodiode array detector was scanned from 190 nm to 300 nm and the detection wavelength was 238 nm. Multiple qualitative analyses were completed according to retention time,full scanning spectrum of photodiode array detector and purity analysis of chromatographic peak. Good linearity was observed in the cyanotoxin concentration range of0.05 mg/L-2. 0 mg/L with correlation coefficients( R) from 0. 9998 to 0. 9999. The limits of detection for10 cyanotoxins were in the range of 0. 005 μg/L-0. 020 μg/L. The recoveries were in the range of 85. 1%-105.3% at the three spiked levels of 0.1 mg/L,1.0 mg/L and 1.8 mg/L with the relative standard deviations( RSD) of 0.8%-9.2%. The method was characterized by wide applicability,convenient operation,quick analytical rate,high sensitivity,good accuracy and high recovery. The qualitative accuracy was improved by using multiple qualitative analyses. This method was successfully applied to determination of 10 kinds of cyanotoxins in lake water.
引文
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20 GB 3838-2002,Environmental Quality Standards for Surface Water.National Standards of the People's Republic of China地表水环境质量标准.中华人民共和国国家标准.GB 3838-2002
21 LIAN Li-Li,GUO Ting-Xiu,WU Yu-Qing,JIN Li,LOU Da-Wei,SUN Da-Zhi.Chinese J.Anal.Chem.,2015,43(12):1876-1881连丽丽,郭亭秀,吴玉清,金丽,娄大伟,孙大志.分析化学,2015,43(12):1876-1881
22 ZHAO Qi-Yue,ZHAO Hong-Shuai,LIU Bao-Xian,LUO Fang.Chinese J.Anal.Chem.,2015,43(4):594-598赵起越,赵红帅,刘保献,骆窻.分析化学,2015,43(4):594-598
23 XU Hui,JIANG Min,WANG Jing.Journal of Instrumental Analysis,2015,34(9):1072-1076许慧,江敏,王婧.分析测试学报,2015,34(9):1072-1076
24 ZHANG Li-Jiang,YIN Li-Hong,PU Yue-Pu,ZHU Guang-Can,LI Xian-Ning,LYU Xi-Wu,Journal of Southeast University(Natural Science Edition),2005,35(3):446-451张立将,尹立红,浦跃朴,朱光灿,李先宁,吕锡武.东南大学学报(自然科学版),2005,35(3):446-451
25 MAO Jing-Ying,YANG Min,DI Yi-An,CAO Jin-Ling,REN Li-Jun,XU Qi-Gong,XI Bei-Dou.Chinese Journal of Environmental Engineering,2012,6(11):3882-3888毛敬英,杨敏,狄一安,曹金玲,任立军,许其功,席北斗.环境工程学报,2012,6(11):3882-3888
2 Xu C,Chen J A,Huang Y J,Qiu Z Q,Luo J H,Zeng H,Zhao Q,Cao J,Shu W Q.Environ.Monit.Assess.,2011,180(1-4):77-86
3 Gurbuz F,Uzunmehmetoglu O Y,Diler,Metcalf J S,Codd G A.Sci.Total Environ.,2016,562:860-868
4 Kyoung-Hee O,Dong-Hwan J,Young-Cheol C.J.Microbiol.,2013,51(1):18-24
5 WANG Yang,LI Yue,FENG Yue,ZHANG A-Mei,XIA Xue-Shan,LIU Li.Chinese Journal of Ecology,2017,36(2):517-523汪洋,李樾,冯悦,张阿梅,夏雪山,刘丽.生态学杂志,2017,36(2):517-523
6 Chrapusta E,Wegrzyn M,Zabaglo K,Kaminski A,Adamski M,Wietrzyk P,Bialczyk J.Toxicon,2015,101:35-40
7 Beltrán E,Ib1ez M,Sancho J V,Hernández F.J.Chromatogr.A,2012,1266(10):61-68
8 Yan S W,Jia A,Merel S,Snyder S A,O'Shea K E,Dionysiou D D,Song W H.Environ.Sci.Technol.,2016,50(3):1437-1446
9 LI Ting,ZHU Wei-Ping,LIU Chun-Hui.China Measurement&Test,2015,41(2):42-45李婷,朱卫平,柳春晖.中国测试,2015,41(2):42-45
10 LAN Ji-Rong,YANG An-Ping,WU Lai-Yan,WANG Song-Bo,JIANG Juan-Juan,WANG Xue-Wu.Journal of Instrumental Analysis,2015,34(6):664-669蓝际荣,杨安平,吴来燕,王松波,蒋娟娟,王学武.分析测试学报,2015,34(6):664-669
11 Li W,Chen J,Xie P,He J,Guo X C,Tuo X,Zhang W,Wu L Y.Aquat.Toxicol.,2014,147:18-25
12 Srivastava A,Singh S,Ahn C Y,Oh H M,Asthana R K.Environ.Sci.Technol.,2013,47(16):8999-9013
13 LIU Yang,HU Pei-Ru,MA Si-San,YE Jin-Yun.J.Lake Sci.,2016,28(2):246-252刘洋,胡佩茹,马思三,叶金云.湖泊科学,2016,28(2):246-252
14 ZHANG Ming,TANG Fang-Liang,XU Jian-Fen,CHEN Feng,YU Bo,WANG Xiao-Dong,YAO Jian-Liang.Environmental Chemistry,2013,32(6):1096-1097张明,唐访良,徐建芬,陈峰,余波,汪晓东,姚建良.环境化学,2013,32(6):1096-1097
15 Li Y W,Zhan X J,Xiang L,Deng Z S,Huang B H,Wen H F,Sun T F,Cai Q Y,Li H,Mo C H.J.Agric.Food Chem.,2014,62(49):11831-11839
16 WANG Yan-Long,CHEN Jun-Hui,GAO Li-Yuan,WANG Shuai,ZHENG Xiao-Ling,SUN Cheng-Jun,WANG Xiao-Ru.Chinese J.Anal.Chem.,2016,44(3):335-341王艳龙,陈军辉,高莉媛,王帅,郑晓玲,孙承君,王小如.分析化学,2016,44(3):335-341
17 Balest L,Murgolo S,Sciancalepore L,Montemurro P,Abis P P,Pastore C,Mascolo G.Anal.Bioanal.Chem.,2016,408(15):4063-4071
18 Edwards C,Lawton L A.J.Chromatogr.A,2010,1217(32):5233-5238
19 World Health Organization,WHO.Guidelines for Drinking Water Quality 4thed,Translated by both Shanghai Municipal Water Supply Controlling and Monitoring Center and Shanghai Jiao Tong University,Shanghai:Shanghai Jiao Tong University Press,2014:263-377世界卫生组织.饮用水水质准则(第四版).上海市供水调度监测中心,上海交通大学译.上海:上海交通大学出版社,2014:263-377
20 GB 3838-2002,Environmental Quality Standards for Surface Water.National Standards of the People's Republic of China地表水环境质量标准.中华人民共和国国家标准.GB 3838-2002
21 LIAN Li-Li,GUO Ting-Xiu,WU Yu-Qing,JIN Li,LOU Da-Wei,SUN Da-Zhi.Chinese J.Anal.Chem.,2015,43(12):1876-1881连丽丽,郭亭秀,吴玉清,金丽,娄大伟,孙大志.分析化学,2015,43(12):1876-1881
22 ZHAO Qi-Yue,ZHAO Hong-Shuai,LIU Bao-Xian,LUO Fang.Chinese J.Anal.Chem.,2015,43(4):594-598赵起越,赵红帅,刘保献,骆窻.分析化学,2015,43(4):594-598
23 XU Hui,JIANG Min,WANG Jing.Journal of Instrumental Analysis,2015,34(9):1072-1076许慧,江敏,王婧.分析测试学报,2015,34(9):1072-1076
24 ZHANG Li-Jiang,YIN Li-Hong,PU Yue-Pu,ZHU Guang-Can,LI Xian-Ning,LYU Xi-Wu,Journal of Southeast University(Natural Science Edition),2005,35(3):446-451张立将,尹立红,浦跃朴,朱光灿,李先宁,吕锡武.东南大学学报(自然科学版),2005,35(3):446-451
25 MAO Jing-Ying,YANG Min,DI Yi-An,CAO Jin-Ling,REN Li-Jun,XU Qi-Gong,XI Bei-Dou.Chinese Journal of Environmental Engineering,2012,6(11):3882-3888毛敬英,杨敏,狄一安,曹金玲,任立军,许其功,席北斗.环境工程学报,2012,6(11):3882-3888