UHPLC-MS/MS Determination of Amyl Xanthic Acid in Water
摘 要
采用超高效液相色谱-串联质谱法测定水中戊基黄原酸的含量。水样(pH 9~10)采用聚四氟乙烯材质的一次性针式过滤器过滤,滤液以ACQUITY UPLC BEH C18色谱柱为分离柱,以不同体积比的水(用氨水调节pH至10)和甲醇混合液为流动相进行梯度洗脱,采用电喷雾负离子源多反应监测模式检测。戊基黄原酸的线性范围为0.500~15.0 μg·L-1,检出限为0.114 μg·L-1。对1.00,8.00,14.0 μg·L-1的戊基黄原酸标准溶液连续测定6次,测定值的相对标准偏差为2.7%~3.9%。以空白样品为基体进行加标回收试验,所得回收率为95.9%~102%。
Abstract
UHPLC-MS/MS was applied to the determination of amyl xanthic acid in water. The water sample (pH 9-10) was filtered with disposable needle filter of PTFE material. ACQUITY UPLC BEH C18 chromatographic column was used as stationary phase, and the mixture of water(pH was adjusted to 10 with ammonia)and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Linearity range of amyl xanthic acid was found between 0.500 μg·L-1 and 15.0 μg·L-1 with detection limit of 0.114 μg·L-1. Precision of the method was tested at the concentration levels of 1.00, 8.00, 14.0μg·L-1 amyl xanthic acid standard solutions for 6 determinations, values of RSD's found were in the range of 2.7%-3.9%. On the base of blank sample, test for recovery was made by standard addition method and values of recovery found were in the range of 95.9%-102%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201711014
所属栏目 工作简报
基金项目
收稿日期 2016/11/1
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联系人作者代佼(cugchem@163.com)
备注夏勇(1983-),男,四川什邡人,工程师,硕士,主要从事环境监测工作
引用该论文: XIA Yong,WANG Haiyan,DAI Jiao. UHPLC-MS/MS Determination of Amyl Xanthic Acid in Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(11): 1308~1312
夏勇,王海燕,代佼. 超高效液相色谱-串联质谱法测定水中戊基黄原酸[J]. 理化检验-化学分册, 2017, 53(11): 1308~1312
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【15】王超,吕怡兵,滕恩江,等.超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J].分析测试学报, 2013,32(1):32-37.
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【2】李辛夫.浮选剂黄药对蛙类胚胎的致畸毒性[J].环境科学学报, 1990,10(2):212-216.
【3】张甫英.浮选剂丁基黄原酸钠对草鱼早期发育阶段的毒性效应[J].水生生物学报, 1995,19(2):104-109.
【4】BOENING D W. Aquatic toxicity and environmental fate of xanthates[J]. Mining Engineering, 1998,(50)9:65-68.
【5】赵玉娥.黄药、黑药、二号油在水体中的降解试验研究[J].黄金, 1995,16(7):47-51.
【6】宋小霞,朱静,张承屏,等.黄药的研制、应用和水污染处理研究进展[J].贵州化工, 2012,37(7):19-22.
【7】BARNES D E, POHLANDT-WATSON C. Separation and determination of the sulph-hydryl flotation collectors using ion-interaction chromatography[J]. Fresenius' Journal of Analytical Chemistry, 1993,345(1):36-42.
【8】ZHOU C S, BAHR A, SCHWEDT G. Studies on the HPLC determination of xanthates via copper (I) xanthates and dixanthogens[J]. Fresenius' Journal of Analytical Chemistry, 1989,334(6):527-533.
【9】ZHOU C S, BAHR A, SCHWEDT G. Separation and determination of xanthates in mixtures as dixanthogens by normal-phase HPLC on a diol-phase[J]. Fresenius' Journal of Analytical Chemistry, 1990,338(8):908-911.
【10】TRUDGETT M. The ultra-trace levels analysis of xanthates by high performance liquid chromatography[D]. New South Wales:University of Western Sydney, 2005.
【11】张蓓蓓,赵永刚,章勇,等.超高效液相色谱-串联质谱法同时测定水体中莠去津和呋喃丹的含量[J].理化检验-化学分册, 2011,47(1):33-35.
【12】熊杰,钱蜀,谢永洪,等.高效液相色谱-串联质谱法同时测定水中丙烯酰胺、苯胺和联苯胺[J].分析化学, 2014,42(1):93-98.
【13】刘景泰,李振国.超高效液相色谱-质谱法测定地表水中丁基黄原酸[J].中国环境监测, 2012,28(5):76-78.
【14】王海燕,夏勇.超高效液相色谱-串联质谱同时测定水中的敌百虫和敌敌畏[J].中国环境监测, 2014,30(6):153-158.
【15】王超,吕怡兵,滕恩江,等.超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J].分析测试学报, 2013,32(1):32-37.
【16】REBELO A M, DOLZAN M D, HELLER M, et al. Simultaneous determination of herbicides in rice by QuECHERS and LC-MS/MS using matrix-matched calibration[J]. Journal of the Brazilian Chemical Society, 2016,27(1):186-193.
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