IC-MS Determination of Etidronic Acid in Cosmetics
摘 要
采用离子色谱-质谱法测定化妆品中羟乙二磷酸的含量。化妆品样品0.500 g,用3.0 mol·L-1乙酸溶液50 mL超声提取15 min,冷却后,用3.0 mol·L-1乙酸溶液定容至100 mL。移取上述溶液10 mL过0.22 μm尼龙滤膜后,再过Oasis HLB固相萃取小柱净化。以IonPac AS11-HC分析柱(250 mm×4 mm)为分离柱,氢氧化钾溶液为淋洗液,采用电喷雾负离子源选择反应监测模式检测。羟乙二磷酸的质量浓度在0.01~5.00 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.5 mg·kg-1。在2.0,4.0,10.0,1 000 mg·kg-1等4个浓度水平进行加标回收试验,回收率为92.0%~103%,测定值的相对标准偏差(n=6)为3.9%~8.1%。
Abstract
IC-MS was applied to the determination of etidronic acid in cosmetics. The cosmetic sample (0.500 g) was extracted ultrasonically with 50 mL of 3.0 mol·L-1 acetic acid solution for 15 min. After cooling, the solution was diluted to 100 mL with 3.0 mol·L-1 acetic acid solution. An aliquot (10 mL) of the above sample solution was taken and filtered on 0.22 μm nylon filtering membrane. The filtrate was purified with Oasis HLB solid phase extraction column. IonPac AS11-HC analytical column (250 mm×4 mm) was used for chromatographic separation, and potassium hydroxide solution was used as eluant. ESI- and the selected reaction monitor mode were adopted in MS. Linear relationship between values of peak area and mass concentration of etidronic acid was kept in the range of 0.01-5.00 mg·L-1, with detection limit (3S/N) of 0.5 mg·kg-1. Tests for recovery were made by standard addition method at 4 concentration levels of 2.0, 4.0, 10.0, 1 000 mg·kg-1, giving values of recovery and RSD's (n=6) in the ranges of 92.0%-103% and 3.9%-8.1% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201805003
所属栏目 工作简报
基金项目 江苏检验检疫局科技计划项目(2017KJ48)
收稿日期 2017/6/29
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备注陈少波,工程师,研究方向为化妆品和食品检测技术,shaobo_chen@yeah.net
引用该论文: CHEN Shaobo,PU Yunyue,XU Zhendong. IC-MS Determination of Etidronic Acid in Cosmetics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(5): 508~511
陈少波,蒲云月,徐振东. 离子色谱-质谱法测定化妆品中羟乙二磷酸[J]. 理化检验-化学分册, 2018, 54(5): 508~511
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【2】NOWACK B. Environmental chemistry of phosphonates[J]. Water Research, 2003,37(11):2533-2546.
【3】LOVDAHL M J, PIETRZYK D J. Anion-exchange separation and determination of bisphosphonates and related analytes by post-column indirect fluorescence detection[J]. Journal of Chromatography A, 1999,850(1/2):143-152.
【4】GB 7916-1987化妆品卫生标准[S].
【5】国家食品药品监督管理总局.化妆品安全技术规范[M].北京:国家食品药品监督管理总局, 2015.
【6】Regulation (EC) No.1223/2009 The European parliament and of the council of 30 November 2009 on cosmetics products[S].
【7】邵青,李士敏,郑琦,等.血浆中羟乙二磷酸钠含量测定方法研究[J].中国药科大学学报, 1997,28(4):222-224.
【8】王秀文,张红梅,刘素艳,等.羟乙二磷酸二钠的电位滴定法测定[J].中国医药工业杂志, 2002,3(3):140-141.
【9】LAND D B, EDMONDS S M. A fluorometric method for determining trace quantities of phosphate[J]. Mikrochimica Acta, 1966,54(6):1013-1023.
【10】MEEK S E, PIETRZYK D J. Liquid chromatographic separation of phosphorus OXO acids and other anions with postcolumn indirect fluorescence detection by aluminum-morin[J]. Analytical Chemistry, 1988,60(14):1397-1400.
【11】景淑华,母昭德,欧阳瑜.荧光淬灭法测定羟乙二磷酸二钠的含量[J].药物分析杂志, 1997,17(2):84-86.
【12】KOVACEVIC M, GARTNER A, NOVIC M. Determination of bisphosphonates by ion chroma-tography-inductively coupled plasma mass spectrometry[J]. Journal of Chromatography A, 2004,1039(1/2):77-82.
【13】丁岚,马强,白桦,等.离子色谱法测定护发和皂类产品中羟乙磷酸及其盐类[J].分析科学学报, 2013,29(5):643-646.
【14】VALLÉE F, MILLER D, LEBE M. Quantitation of etidronic acid in human plasma by GC/MS[J]. Journal of Pharmacy and Pharmaceutical Sciences, 1999,2(2):82-82.
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