高效液相色谱法测定造型黏土中2种防腐剂
HPLC Determination of 2 Preservatives in Moulding Clay
摘 要
提出了高效液相色谱法测定造型黏土中2种防腐剂(2-甲基-4-异噻唑啉-3-酮和5-氯-2-甲基-4-异噻唑啉-3-酮)的方法。黏土样品以甲醇进行超声提取,所得提取液以柱温为35 ℃的Agilent Eclipse XDB-C18色谱柱为分离柱,用甲醇与水以不同比例混合的溶液为流动相进行梯度洗脱,在检测波长275 nm处进行测定。2种防腐剂的质量浓度均在0.50~40 mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)分别为6.80,14.8 μg·L-1。方法用于造型黏土样品分析,加标回收率在90.9%~120%之间,测定值的相对标准偏差(n=6)在0.060%~2.4%之间。
造型黏土
防腐剂
HPLC
Moulding clay
Preservatives
Abstract
A method of HPLC for the determination of 2 preservatives (i.e., 2-methyl-4-isothiazolin-3-on and 5-chloro-2-methyl-4-isothiazolin-3-one) in moulding clay was proposed. The sample was extracted ultrasonically with methanol. The extract was separated by chromatography by using Agilent Eclipse XDB C18 column (at column temp. of 35 ℃) as separation column, and mixtures of methanol and water in various ratios as mobile phase in gradient elution. UV-detection at 275 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 2 preservatives were kept in the same range of 0.50-40 mg·L-1, with detection limits (3S/N) of 6.80, 14.8 μg·L-1 respectively. The proposed method was applied to the analysis of substantial samples. Values of recovery found by standard addition method were in the range of 90.9%-120%, and RSD′s (n=6) found were in the range of 0.060%-2.4%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201602011
所属栏目 工作简报
基金项目 国家质检总局风险监测任务(监测中心［2015］7号)
收稿日期 2015/7/27
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备注彭姚珊(1990-),女,四川泸州人,硕士研究生,主要 从事消费品有毒有害物质的检测研究。
引用该论文: PENG Yao-shan,GAO Jun-wei,WANG Ai-xia,ZHOU Tian-xiao,LIU Pan,ZHU Ning-ning. HPLC Determination of 2 Preservatives in Moulding Clay[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(2): 171～175
彭姚珊,高俊伟,王爱霞,周天啸,刘盼,祝宁宁. 高效液相色谱法测定造型黏土中2种防腐剂[J]. 理化检验－化学分册, 2016, 52(2): 171～175
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参考文献
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【2】CELEIRO M, GUERRA E, PABLO LAMAS J, et al. Development of a multianalyte method based on micro-matrix-solid-phase dispersion for the analysis of fragrance allergens and preservatives in personal care products［J］. Journal of Chromatography A, 2014,1344:1-14.
【3】ALVAREZ-RIVERA G, VILA M, LORES M, et al. Development of a multi-preservative method based on solid-phase microextraction-gas chromatography-tandem mass spectrometry forcosmetic analysis［J］. Journal of Chromatography A, 2014,1339:13-25.
【4】李晶,徐济仓,魏玉玲,等.超高效液相色谱法测定植物提取物中6种防腐剂含量［J］.理化检验-化学分册, 2013,49(8):965-967.
【5】罗晶,施法,陈晓辉,等.HPLC法同时测定抗病毒口服液中4种防腐剂［J］.西北药学杂志, 2012,27(1):36-38.
【6】沈燕琼,杨丽英,舒丽丹,等.气相色谱-质谱法测定感冒颗粒中7种防腐剂［J］.理化检验-化学分册, 2013,49(8):937-939.
【7】ZHOU X, CAO S R, LI X L, et al. Simultaneous determination of 18 preservative residues in vegetables by ultra high performance liquid chromatography coupled with triple quadrupole/linear ion trap mass spectrometry using a dispersive-SPE procedure［J］. Journal of Chromatography B, 2015,989:21-26.
【8】MARTN J, SANTOS J L, APARICIO I, et al. Determination of hormones, aplasticizer, preservatives, per-fluoroalkylated compounds, and a flame retardant in water samples by ultrasound-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic drop［J］. Talanta, 2015,143:335-343.
【9】ZHU K X, GONG S G, DAI Y H, et al. Determination of preservatives in water-based adhesives by gas chromatography-mass spectrometry［J］. Analytical Letters, 2015,48:1396-1410.
【10】苏建国.高效液相色谱法测定豆制品中2种甜味剂和7种防腐剂［J］.理化检验-化学分册, 2013,49(1):26-28.
【11】KOH B R D, KIM J Y, JANG M S, et al. Simultaneous determination of preservatives in sausages using liquid chromatography with electrospray ionization tandem mass spectrometry［J］. Korean J Vet Serv, 2015,38:127-136.
【12】SUN B B, QI L, WANG M L. Determination of preservatives in soft drinks by capillary electrophoresis with ionic liquids as the electrolyte additives［J］. J Sep Sci, 2014,37:2248-2252.
【13】王改香,张磊,唐晓军,等.气相色谱-质谱法测定化妆品中10种防腐剂［J］.理化检验-化学分册, 2015,51(1):35-38.
【14】CELEIRO M, LAMAS J P, GARCIA-JARES C, et al. Pressurized liquid extraction-gas chromatography-mass spectrometry analysis of fragrance allergens, musks, phthalates and preservatives in baby wipes［J］. Journal of Chromatography A, 2015,1384:9-21.
【15】ALVAREZ-RIVERA G, DAGNAC T, LORES M, et al. Determination of isothiazolinone preservatives in cosmetics and household products by matrix solid-phase dispersion followed by high-performance liquid chromatography-tandem mass spectrometry［J］. Journal of Chromatography A, 2012,1270:41-50.
【16】ROSERO-MOREANO M, CANELLAS E, NERN C. Three-phase hollow-fiber liquid-phase microextraction combined with HPLC-UV for the determination of isothiazolinone biocides in adhesives used for food packaging materials［J］. J Sep Sci, 2014,37:272-280.
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