HPLC Determination of Boric Acid and Borax in Essence and Perfume with Precolumn Derivatization
摘 要
香精香料样品中的硼酸经姜黄素的乙酸溶液在室温下进行衍生化,所得硼的衍生物用高效液相色谱法分析。选用Hypersil ODS2色谱柱(4.6 mm×250 mm,5 μm)为固定相,以甲醇与0.012 mol·L-1四丁基溴化铵(TBABr)溶液按体积比80比20混合所得溶液为流动相进行淋洗,于波长550 nm处进行检测。根据硼砂在硫酸环境下定量转化成硼酸的原理间接测定硼砂。硼的色谱峰面积与其质量浓度在0.004~0.2 mg·L-1范围内呈线性关系,检出限(3s)为4.0×10-4mg·L-1。在3个浓度水平下做加标回收试验,所得硼酸和硼砂的平均回收率分别在92.1%~106.6%和92.9%~107.1%之间。
Abstract
Boric acid in samples of essence and perfume was derivatized with curcumin (dissolved in acetic acid) at room temperature. The derivatized product of boron was used for HPLC analysis, using Hypersil ODS2 chromatographic column (4.6 mm×250 mm, 5 μm) as stationary phase and mixtures of methanol and 0.012 mol·L-1 TBABr (80+20) as mobile phase. Based on the quantitative conversion of borax into boric acid in sulfuric acid medium, borax was determined by indirect determination of boric acid. Linear relationship was found between values of peak area determined at wavelength of 550 nm and mass concentration of boron in the range of 0.004-0.2 mg·L-1, with detection limit (3s) of 4.0×10-4mg·L-1. Tests for recovery were performed by standard addition method at 3 concentration levels; results of recovery of boric acid and borax found were in the ranges of 92.1%-106.6% and 92.9%-107.1% respectively.
中图分类号 O657.7
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收稿日期 2010/11/26
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联系人作者周示玉(lzg@zjut.edu.cn)
备注周示玉(1986-),男,贵州贵阳人,硕士研究生,主要研究方向为食品分析。
引用该论文: ZHOU Shi-yu,JIANG Jian,ZHOU Guo-jun,HU Bao-xiang,LI Zu-guang. HPLC Determination of Boric Acid and Borax in Essence and Perfume with Precolumn Derivatization[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(2): 219~221
周示玉,蒋健,周国俊,胡宝祥,李祖光. 柱前衍生-高效液相色谱法测定香精香料中硼酸和硼砂[J]. 理化检验-化学分册, 2012, 48(2): 219~221
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【2】曹艇,刘梦溪.食品中非法添加硼砂的危害[J].中国预防医学杂志, 2003,4(3):237-238.
【3】何福德,黎伯东,劳成涌,等.灵山县部分传统食品中掺加硼砂情况的调查[J].中国卫生检验杂志, 2008,18(12):2734-2791.
【4】SPICER S, STRICKLAND H. Determination of microgram and sub-microgram amounts of boron absorptiometric determination using curcumin[J]. Anal Chim Acta, 1958,18:231-239.
【5】GROTHEE W. Spectrophotometric determination of boric acid in boron powder with curcumin[J]. Anal Chem, 1979,51(14):2402-2403.
【6】YOSHIDA M, WATABIKI T, ISHIDA N. Spectrophotometric determination of boric acid by the curcumin method[J]. Nihon Hoigaku Zasshi, 1989,43(6):490-496.
【7】杨柳,吴文岗.食品中硼砂的检验方法[J].理化检验-化学分册, 2008,44(8):795-806.
【8】LEWIS D T. The polarographic determination of boron[J]. Analyst, 1956,81(966):531-531.
【9】李晓明,邓毓芳,陆光汉.粮食中微量硼的极谱测定[J].理化检验-化学分册, 1994,30(5):288-290.
【10】隋迎军,杜志茂,冯春堂,等.高效液相色谱法测定冰硼散中硼砂的含量[J].解放军药学学报, 2002,18(2):125-125.
【11】陈艳,李红光.食品中硼砂的反相高效液相色谱测定法[J].环境与健康杂志, 2007,24(12):994-995.
【12】RADHIKA R, SURESH A. Determination of boron at sub-ppm levels in uranium oxide and aluminum by hyphenated system of complex formation reaction and high-performance liquid chromatography[J]. Talanta, 2008,75:585-588.
【13】陆建平,彭剑.火焰原子吸收光谱法间接测定钢中硼量[J].理化检验-化学分册, 2008,44(12):1204-1212.
【14】SAH N, BROWN P H. Boron determination-A review of analytical methods[J]. Microchem J, 1997,56(3):294-296.
【15】胡小玲,黄辉涛,肖学成.ICP-AES法测定食品中硼砂[J].中国卫生检验杂志, 2008,18(10):1994-1995.
【16】陈安明.电感耦合等离子体发射光谱发测定低合金钢中痕量硼[J].理化检验-化学分册, 2007,43(8):644-646.
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