HPLC Determination of Resin Acids in Adhesives
摘 要
样品2.500 g溶解于乙酸乙酯5 mL中,加入甲醇15 mL涡旋0.5 min,再以6 000 r·min-1转速离心10 min,用甲醇冲洗离心管及沉淀,合并上清液和洗涤液,并定容至25 mL。上述所得溶液以Waters XTerra RP18色谱柱为固定相,乙腈-0.4%(体积分数)乙酸溶液(80+20)混合液为流动相进行高效液相色谱分离。脱氢枞酸、枞酸及其同分异构体的检测波长分别为200,216 nm。树脂酸的质量浓度在1.0~100.0 mg·L-1范围内与其峰面积呈线性关系,脱氢枞酸、枞酸及其同分异构体的测定下限(10S/N)分别为3.0,10.0 mg·kg-1。按标准加入法进行回收试验,回收率在91.9%~98.0%之间,相对标准偏差(n=6)在0.26%~2.8%之间。
Abstract
The sample (2.500 g) was dissolved in 5 mL of ethyl acetate, and 15 mL of methanol was added into the solution to whirl for 0.5 min. The mixture was centrifuged at rate of 6 000 r·min-1 for 10 min, and the centrifuge tube and sedimentation were washed by methanol. The supernatant and washing solution were combined and made its volume up to 25 mL. The above solution obtained was separated by HPLC using Waters XTerra RP18 column as the stationary phase and a mixture of acetonitrile-0.4% (φ) acetic acid solution (80+20) as the mobile phase. Detection wavelengths were 200 nm for dehydroabietic acid and 216 nm for abietic acid isomers. Linear relationships between values of peak area and mass concentration of resin acids were obtained in the range of 1.0-100.0 mg·L-1, with lower limits of determination (10S/N) of 3.0 mg·kg-1 for dehydroabietic acid and 10.0 mg·kg-1 for abietic acid isomers. Test for recovery was made by standard addition method, giving results in the range of 91.9%-98.0%, with RSDs (n=6) ranged from 0.26% to 2.8%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201801005
所属栏目 工作简报
基金项目 质检总局科研项目(2015IK212);国家认监委科研制标项目(2015B074);山东省重点研发计划(2017GSF20116)
收稿日期 2016/12/23
修改稿日期
网络出版日期
作者单位点击查看
备注王乐(1982-),女,山东淄博人,高级工程师,研究方向为食品及食品接触制品品质研究与分析,dingshenyong@163.com
引用该论文: WANG Le,XIANG Haibo,TAO Lin,ZHANG Aixia,CHEN Xi,HE Guihua,ZHENG Xinhua. HPLC Determination of Resin Acids in Adhesives[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(1): 24~30
王乐,项海波,陶琳,张爱霞,陈晞,何桂华,郑新华. 高效液相色谱法测定胶黏剂中树脂酸的含量[J]. 理化检验-化学分册, 2018, 54(1): 24~30
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】朱际善,张之平,沈雪珍,等.松香合成水溶性塑料薄膜胶粘剂的研究[J].林产化学与工业, 1994(增刊1):27-30.
【2】徐嵘,王成云,武书彬,等.纸质食品包装材料中松香酸含量测定抽提方案的优化[J].食品安全质量检测学报, 2014,5(11):3556-3563.
【3】崔渤.塑料复合软包装胶黏剂市场研究[J].塑料与包装, 2010(4):20-21.
【4】朱蕾,张俭波,张泓,等.食品接触用粘合剂法规管理模式分析[J].包装工程, 2015(1):46-50.
【5】郭新东,冼燕萍,杜志峰,等.气相色谱法快速测定食品包装用胶粘剂中的9种有害物质[J].现代食品科技, 2008,24(9):937-939.
【6】宋湛谦.松香的精细化工利用(Ⅰ)——松香的组成与性质[J].林产化工通讯, 2002,36(4):29-33.
【7】SERREQI A N, GAMBOA H, STARK K, et al. Resin acid markers for total resin acid content of in-mill process lines of a TMP/CTMP pulp mill[J]. Water Research, 2000,34(5):1727-1733.
【8】OZAKI A, OOSHIMA T, MORI Y. Migration of dehydroabietic and abietic acids from paper and paperboard food packaging into food-simulating solvents and Tenax TA[J]. Food Additives and Contaminants, 2006,23(8):854-860.
【9】TAVENDALE M H, MCFARLANE P N, MACKIE K L, et al. The fate of resin acids-1. The biotransformation and degradation of deuterium labelled dehydroabietic acid in anaerobic sediments[J]. Chemosphere, 1997,35(10):2137-2151.
【10】SÖDERBERG T A, JOHANSSON A, GREF R. Toxic effects of some conifer resin acids and tea tree oil on human epithelial and fibroblast cells[J]. Toxicology, 1996,107(2):99-109.
【11】OZAKI A, YAMAGUCHI Y, FUJITA T, et al. Safety assessment of paper and board food packaging: Chemical analysis and genotoxicity of possible contaminants in packaging[J]. Food Additives and Contaminants, 2005,22(10):1053-1060.
【12】汪杨丽,苏晶,张毅.舒筋活血丸中非法添加物松香酸的检测方法[J].中国现代中药, 2015,17(3):244-246.
【13】ISO/TR 16178:2012 Footwear-critical substances potentially present in footwear and footwear components[S].
【14】黄小泳,徐明全.GC检测松香产品的有机酸含量[J].现代食品与药品杂志, 2006,16(6):28-29.
【15】段文贵,陈小鹏,周永红.自制氢化松香主要化学组成的GC-MS法测定[J].分析测试学报, 2003,22(1):5-8.
【16】MARINACH C, PAPILLON M C, PEPE C. Identification of binding media in works of art by gas chromatography-mass spectrometry[J]. Journal of Cultural Heritage, 2004,5(2):231-240.
【17】张苏珍,耿志明,王道营,等.固相萃取-高效液相色谱法检测肉鸭表皮组织中的松香酸[J].食品科学, 2014,35(4):82-85.
【18】王英锋,魏小燕.HPLC测定枫香脂碱提物中脱氢松香酸和松香酸的含量[J].中国中药杂志, 2013,38(1):57-59.
【19】陈安珍,沙启营,单秀明,等.跌打片中松香酸的HPLC和HPLC-MS/MS检测方法研究[J].中成药, 2013,35(9):1940-1942.
【20】张妤琳,曹玲,谭力,等.液质联用技术用于沉香中非法掺入含松香酸类物质的检测[J].中成药, 2011,33(5):844-847.
【21】董清木,林睿,赖莺,等.高效液相色谱法测定建筑用胶黏剂中的游离苯酚[J].广州化学, 2013,38(3):29-33.
【22】周晓,李小兰,陈志燕,等.高效液相色谱法测定水基胶黏剂中3种异噻唑啉酮类杀菌剂[J].色谱, 2015,33(1):75-79.
【23】叶曦雯,王芹,牛增元,等.高效液相色谱法检测压敏胶及其制品中的防老剂D[J].分析测试学报, 2011,30(9):1023-1027.
【24】南京林产工业学院松香结晶研究组.树脂酸组成和松香结晶[J].南京林产土业学院学报, 1980(2):1-14.
【25】宋湛谦.马尾松松香中混杂湿地松松香的检测方法[J].林产化学与工业, 2005,25(增刊1):137-138.
【26】SONG Z, LIANG Z, XING L. Chemical characteristics of oleoresins from Chinese pine species[J]. Biochemical Systematics and Ecology, 1995,23(5):517-522.
【2】徐嵘,王成云,武书彬,等.纸质食品包装材料中松香酸含量测定抽提方案的优化[J].食品安全质量检测学报, 2014,5(11):3556-3563.
【3】崔渤.塑料复合软包装胶黏剂市场研究[J].塑料与包装, 2010(4):20-21.
【4】朱蕾,张俭波,张泓,等.食品接触用粘合剂法规管理模式分析[J].包装工程, 2015(1):46-50.
【5】郭新东,冼燕萍,杜志峰,等.气相色谱法快速测定食品包装用胶粘剂中的9种有害物质[J].现代食品科技, 2008,24(9):937-939.
【6】宋湛谦.松香的精细化工利用(Ⅰ)——松香的组成与性质[J].林产化工通讯, 2002,36(4):29-33.
【7】SERREQI A N, GAMBOA H, STARK K, et al. Resin acid markers for total resin acid content of in-mill process lines of a TMP/CTMP pulp mill[J]. Water Research, 2000,34(5):1727-1733.
【8】OZAKI A, OOSHIMA T, MORI Y. Migration of dehydroabietic and abietic acids from paper and paperboard food packaging into food-simulating solvents and Tenax TA[J]. Food Additives and Contaminants, 2006,23(8):854-860.
【9】TAVENDALE M H, MCFARLANE P N, MACKIE K L, et al. The fate of resin acids-1. The biotransformation and degradation of deuterium labelled dehydroabietic acid in anaerobic sediments[J]. Chemosphere, 1997,35(10):2137-2151.
【10】SÖDERBERG T A, JOHANSSON A, GREF R. Toxic effects of some conifer resin acids and tea tree oil on human epithelial and fibroblast cells[J]. Toxicology, 1996,107(2):99-109.
【11】OZAKI A, YAMAGUCHI Y, FUJITA T, et al. Safety assessment of paper and board food packaging: Chemical analysis and genotoxicity of possible contaminants in packaging[J]. Food Additives and Contaminants, 2005,22(10):1053-1060.
【12】汪杨丽,苏晶,张毅.舒筋活血丸中非法添加物松香酸的检测方法[J].中国现代中药, 2015,17(3):244-246.
【13】ISO/TR 16178:2012 Footwear-critical substances potentially present in footwear and footwear components[S].
【14】黄小泳,徐明全.GC检测松香产品的有机酸含量[J].现代食品与药品杂志, 2006,16(6):28-29.
【15】段文贵,陈小鹏,周永红.自制氢化松香主要化学组成的GC-MS法测定[J].分析测试学报, 2003,22(1):5-8.
【16】MARINACH C, PAPILLON M C, PEPE C. Identification of binding media in works of art by gas chromatography-mass spectrometry[J]. Journal of Cultural Heritage, 2004,5(2):231-240.
【17】张苏珍,耿志明,王道营,等.固相萃取-高效液相色谱法检测肉鸭表皮组织中的松香酸[J].食品科学, 2014,35(4):82-85.
【18】王英锋,魏小燕.HPLC测定枫香脂碱提物中脱氢松香酸和松香酸的含量[J].中国中药杂志, 2013,38(1):57-59.
【19】陈安珍,沙启营,单秀明,等.跌打片中松香酸的HPLC和HPLC-MS/MS检测方法研究[J].中成药, 2013,35(9):1940-1942.
【20】张妤琳,曹玲,谭力,等.液质联用技术用于沉香中非法掺入含松香酸类物质的检测[J].中成药, 2011,33(5):844-847.
【21】董清木,林睿,赖莺,等.高效液相色谱法测定建筑用胶黏剂中的游离苯酚[J].广州化学, 2013,38(3):29-33.
【22】周晓,李小兰,陈志燕,等.高效液相色谱法测定水基胶黏剂中3种异噻唑啉酮类杀菌剂[J].色谱, 2015,33(1):75-79.
【23】叶曦雯,王芹,牛增元,等.高效液相色谱法检测压敏胶及其制品中的防老剂D[J].分析测试学报, 2011,30(9):1023-1027.
【24】南京林产工业学院松香结晶研究组.树脂酸组成和松香结晶[J].南京林产土业学院学报, 1980(2):1-14.
【25】宋湛谦.马尾松松香中混杂湿地松松香的检测方法[J].林产化学与工业, 2005,25(增刊1):137-138.
【26】SONG Z, LIANG Z, XING L. Chemical characteristics of oleoresins from Chinese pine species[J]. Biochemical Systematics and Ecology, 1995,23(5):517-522.
相关信息