干旱区生态环境知识资源中心(Arid): 超高效液相色谱 -串联质谱法快速检测地表水中12种微囊藻毒素

Arid

	超高效液相色谱 -串联质谱法快速检测地表水中12种微囊藻毒素
其他题名	Simultaneous rapid determination of 12 microcystins in surface water with ultra performance liquid chromatography-tandem mass spectrometry
	王军淋; 张京顺; 胡争艳; 张念华; 冯靓; 王志园; 姚燕红; 蔡增轩
来源期刊	中国公共卫生
ISSN	1001-0580
出版年	2021
卷号	37 期号:6 页码:1001-0580
中文摘要	目的建立超高效液相色谱 -串联质谱法快速检测地表水中的12种微囊藻毒素(MCs)方法,为地表水快速检测提供依据。方法水样冻融3次后,经玻璃纤维滤膜过滤,直接进样分析,若有MCs低于定量限,将冻融后水样过玻璃纤维滤纸(GF/C),采用HLB柱富集,40 %甲醇水淋洗,甲醇洗脱后经等比例水稀释,混合纤维滤膜过滤后进样分析。以0.2 %甲酸水溶液和0.2 %甲酸甲醇 -乙腈溶液(40 + 60)作为流动相进行梯度洗脱,采用ACQUITY UPLC BEH C18柱(100 mm*2.1 mm,1.7 mum)分离,正离子模式下多反应监测(MRM)检测,外标法定量。结果12种MCs在0.1~5.0 ng/mL范围内线性关系良好,相关系数均 > 0.995;方法检出限为0.03~0.06 mug/L(直接进样法)、 0.006~0.012 mug/L(SPE法),回收率为83.07 %~108.27 %,相对标准偏差为0.46 %~12.76 %(n = 6)。采用所建方法对6份实际样品进行检测,在4份地表水中检测到多种MCs。结论超高效液相色谱 -串联质谱法操作简单、灵敏度高、选择性好,适用于地表水中12种MCs的快速检测。
英文摘要	Objective To establish a rapid method for simultaneous determination of 12 microcystins in surface water with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Surface water samples were firstly freeze-thawing for three times, then directly filtered with glass fiber filters for injection. When several or one of the microcystins under the concentration of relevant limit of quantification, GF/C glass fiber was used for filter and an Oasis HLB SPE column was used for the concentration and purifying. The 40% methanol aqueous solution was used for washing; after elution with methanol, equal volume of ultrapure water was added for dilution, and then filtered through synthetic fabric membrane for injection. The separation of the analytes was carried out on an ACQUITY UPLC BEH C18 column (100 mm*2.1 mm, 1.7 mum) with gradient elution using bobile phases of 0.2% (v/v) formic acid aqueous solution and methanol mix with acetonitrile at ratio of 2 to 3 containing 0.2% (v/v) formic acid. The 12 microcystins were detected with positive electrospray ionization in multiple reaction monitoring modes, and quantified by external standard methods. Toxicity equivalent factor conversion was used for total toxicity analysis of the detected microcystins. Results The linear ranges of 12 microcystins were 0.1 - 5.0 ng/mL and the correlation coefficients were greater than 0.995. The limits of detection and quantification were 0.006 - 0.012 mug/L and 0.02 - 0.04 mug/L for SPE method and 0.03 - 0.06 mug/L and 0.1 - 0.2 mug/L for direct injection, respectively. The recoveries were in the range of 83.07% - 108.27% with the relative standard deviations ranging from 0.46% - 12.76% (n = 6). Then the established method was used for the determination of 6 surface water samples and several kinds of microcystins were detected in 4 of the samples. Conclusion The established method is rapid, simple, sensitive and accurate, and could be applied in determination of 12 microcystins in surface water.
中文关键词	超高效液相色谱 -串联质谱 ; 微囊藻毒素(MCs) ; 直接进样 ; 固相萃取 ; 地表水
英文关键词	ultra performance liquid chromatography-tandem mass spectrometry microcystins direct injection solid phase extraction surface water
类型	Article
语种	中文
国家	中国
收录类别	CSCD
WOS类目	Public, Environmental & Occupational Health
CSCD记录号	CSCD:6997082
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/365421
作者单位	王军淋, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 张京顺, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 胡争艳, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 张念华, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 冯靓, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 王志园, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 姚燕红, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.; 蔡增轩, 浙江省疾病预防控制中心, 杭州, 浙江 310051, 中国.
推荐引用方式 GB/T 7714	王军淋,张京顺,胡争艳,等. 超高效液相色谱 -串联质谱法快速检测地表水中12种微囊藻毒素[J],2021,37(6):1001-0580.
APA	王军淋.,张京顺.,胡争艳.,张念华.,冯靓.,...&蔡增轩.(2021).超高效液相色谱 -串联质谱法快速检测地表水中12种微囊藻毒素.中国公共卫生,37(6),1001-0580.
MLA	王军淋,et al."超高效液相色谱 -串联质谱法快速检测地表水中12种微囊藻毒素".中国公共卫生 37.6(2021):1001-0580.