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浙江大学学报(理学版)  2019, Vol. 46 Issue (3): 333-338    DOI: 10.3785/j.issn.1008-9497.2019.03.011
化学     
离子色谱法同时测定植物生长调节剂中氯化胆碱、甲哌鎓及N-甲基哌啶
朱作艺1, 张玉1, 王君虹1, 李雪1, 王伟1,2,3, 孙彬4
1.浙江省农业科学院农产品质量标准研究所,浙江 杭州 310021
2.农产品质量安全国家重点实验室省部共建培育基地,浙江 杭州 310021
3.农业部创意农业重点实验室,浙江 杭州 310021
4.武义中正食品检测有限公司,浙江 金华 321200
Ion chromatographic method for simultaneous measurement of choline chloride, mepiquat chloride and N-methylpiperidine in plant growth regulators
Zuoyi ZHU1, Yu ZHANG1, Junhong WANG1, Xue LI1, Wei WANG1,2,3, Bin SUN4
1.Institute of Quality and Standard for Agricultural Products, Zhejiang Academy of Agricultural Science, Hangzhou 310021, China
2.State Key Laboratory of Quality and Safety for Agricultural Products Co-Founded by Zhejiang Province and Ministry of Agriculture, Hangzhou 310021, China
3.Key Laboratory of Creative Agriculture, Ministry of Agriculture, Hangzhou 310021, China
4.Wuyi Zhongzheng Food Testing Co. LTD., Jinhua 321200, Zhejiang Province,China
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摘要: 建立了一种离子色谱-抑制电导同时测定植物生长调节剂中主要活性成分氯化胆碱、甲哌鎓以及杂质N-甲基哌啶的快速检测方法。 样品经稀释过膜后直接进样分析, 采用阳离子交换色谱柱thermo scientific ionpac CG17 (50 mm×4 mm) + CS17 (250 mm×4 mm),以10 mmol·L-1甲烷磺酸溶液等度淋洗,可在10 min内完成以上目标分析物的检测,且常规阳离子(Li+、 Na+、 NH4+、 K+、 Mg2+和Ca2+)不会干扰对3种化合物的测定。 在优化后的最佳色谱条件下,氯化胆碱的线性范围为0.1~500 mg·L-1,甲哌鎓的线性范围为0.5~500 mg·L-1,N-甲基哌啶的线性范围为0.4~200 mg·L-1,3种化合物线性相关系数(r)均大于0.999 4,线性关系良好。 3种目标分析物的检出限(信噪比S/N = 3)为28.0~112.5 μg·L-1,定量限(信噪比S/N = 10)为93.5~375.0 μg·L-1,峰面积的相对标准偏差(RSD, n = 6)均小于0.47%,表明方法具有较好的重现性。 该检测方法简单方便,已成功应用于商品化植物生长调节剂中3种成分质量浓度的测定,实际样品加标回收率为96.0%~103.6%。 可应用于相关植物生长调节剂原料及成品的质量控制。
关键词: 氯化胆碱甲哌鎓N-甲基哌啶离子色谱植物生长调节剂    
Abstract: This paper presents a rapid and simple method for simultaneous measure of the main active components choline chloride, mepiquat chloride, and the impurity N-methylpiperidine in plant growth regulators using ion chromatography with suppressed conductivity detection. According to this method,the samples are diluted in deionized water and then undergo a process of membrane filtration. The filtrate is directly injected into an ion chromatograph equipped with a commercially available cation-exchange column Thermo Scientific Ionpac CS17 (250 mm × 4 mm). The determination of target analytes can be finished in less than 10 min with an isocratic eluent consisting of 10 mmol·L-1 methane sulfonic acid (MSA), and no interferences exist between common cations (Li+, Na+, NH4+, K+, Mg2+ and Ca2+) and target analytes. Under the optimal conditions, the proposed method shows good linearity in the range from 0.1 to 500 mg·L-1 for choline chloride, from 0.5 to 500 mg·L-1 for mepiquat chloride and from 0.4 to 200 mg·L-1 for N-methylpiperidine, with correlation coefficients (r) ≥ 0.999 4. Limits of detection (LODs, S/N = 3) are in the range from 28.0 to 112.5 μg·L-1 and Limits of quantitation (LOQs, S/N = 10) are in the range from 93.5 to 375.0 μg·L-1.It also has a good repeatability (RSDs ≤ 0.47%, n = 6). This method has been successfully applied to rapid and simultaneous analysis of the three compounds in commercial plant growth regulators. The overall average recoveries range from 96.0% to 103.6%. The proposed method can be applied to the quality control of raw materials and commercial products of plant growth regulator.
Key words: choline chloride    mepiquat chloride    N-methylpiperidine    ion chromatography    plant growth regulator
收稿日期: 2018-04-11 出版日期: 2019-05-25
CLC:  O657.7  
基金资助: 浙江省科技计划项目 (2018C02057).
通讯作者: ORCID:http:// orcid.org/0000-0003-4583-6605 ,E-mail: wangwei5228345@163.com.     E-mail: wangwei5228345@163.com.
作者简介: 朱作艺(1987―),ORCID:http://orcid.org/0000-0002-5295-0804,女,博士,主要从事农产品质量安全检测研究.
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引用本文:

朱作艺, 张玉, 王君虹, 李雪, 王伟, 孙彬. 离子色谱法同时测定植物生长调节剂中氯化胆碱、甲哌鎓及N-甲基哌啶[J]. 浙江大学学报(理学版), 2019, 46(3): 333-338.

Zuoyi ZHU, Yu ZHANG, Junhong WANG, Xue LI, Wei WANG, Bin SUN. Ion chromatographic method for simultaneous measurement of choline chloride, mepiquat chloride and N-methylpiperidine in plant growth regulators. Journal of ZheJIang University(Science Edition), 2019, 46(3): 333-338.

链接本文:

https://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2019.03.011        https://www.zjujournals.com/sci/CN/Y2019/V46/I3/333

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