表面增强拉曼光谱测定保健品中非法添加物西地那非
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摘要
基于表面增强拉曼光谱技术(SERS),采用自制表面增强试剂(纳米金)与厂家提供的表面增强试剂,对比研究了对21种查缴的保健品样品中的非法添加物西地那非的快速拉曼检测效果,同时考察了不同配比纳米金和不同浓度的盐酸、硝酸和硫酸作为助剂的增强效果。结果表明,自制纳米金表面增强试剂(氯金酸和柠檬酸钠的体积比1∶1)及2.67 mol·L~(-1)的硝酸表面增强效果为佳,可对浓度为0.01μg·mL~(-1)西地那非阳性检出;与飞行时间-液质联用仪(QTOF-LC-MS)分析结果对比,自制纳米金检测吻合度为100%,厂家提供的增强试剂检测吻合度为86.4%。综上,自制表面增强试剂(纳米金)表面增强效果不差于厂家提供的表面增强试剂。
Based on surface-enhanced raman spectroscopy(SERS),the illegal additive sildenafil in 21 samples of seized health care products was detected by self-made nano-gold as the surface-enhanced reagents comparing with those provided by the manufacturers. The enhancement effects of nano-gold in various proportions with using diverse concentrations of hydrochloric acid,nitric acid and sulfuric acid were additionally measured. The results showed that:As the minimum detection limit of sildenafil was 0.01 μg·mL~(-1),the enhancement effect of self-made nano-gold as the surface-enhanced reagent(the volume of cholor-gold acid and sodium citrate was in the proportion 1∶1)added nitric acid with the concentration of 2.67 mol·L~(-1) was as result the best among the all tests,so that it was 100% consistent with the results analyzed by QTOF-LC-MS,while those provided by the manufacturer were only 86.4% consistent. This indicated that the surface enhancement effect of the self-made surface enhancement reagent(nano-gold)was not inferior to that provided by the manufacturer.
Based on surface-enhanced raman spectroscopy(SERS),the illegal additive sildenafil in 21 samples of seized health care products was detected by self-made nano-gold as the surface-enhanced reagents comparing with those provided by the manufacturers. The enhancement effects of nano-gold in various proportions with using diverse concentrations of hydrochloric acid,nitric acid and sulfuric acid were additionally measured. The results showed that:As the minimum detection limit of sildenafil was 0.01 μg·mL~(-1),the enhancement effect of self-made nano-gold as the surface-enhanced reagent(the volume of cholor-gold acid and sodium citrate was in the proportion 1∶1)added nitric acid with the concentration of 2.67 mol·L~(-1) was as result the best among the all tests,so that it was 100% consistent with the results analyzed by QTOF-LC-MS,while those provided by the manufacturer were only 86.4% consistent. This indicated that the surface enhancement effect of the self-made surface enhancement reagent(nano-gold)was not inferior to that provided by the manufacturer.
引文
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[17]刘燕德,张宇翔,王海阳.脐橙表皮两种混合农药残留的表面增强拉曼光谱定量检测[J].光谱学与光谱分析,2018,38(1):123-127.
[18]王乐,张爱霞,陈晞,郑新华,等.表面增强拉曼光谱法快速检测饮料中玫瑰红B[J].食品研究与开发,2018,39(7):126-130.
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[20]王学良,冯艳春,胡昌勤.近红外特征谱段相关系数法测定中药胶囊中添加枸橼酸西地那非[J].分析化学,2009,37(12):1825-1828.
[21]王红梅,李玲玲,陈海滨,等.表面增强拉曼光谱对西地那非类药物的快速检测[J].高等学校化学学报,2017,38(6):1040-1045.
[22]刘元瑞,葛海生,赵康虎,等.薄层原位表面增强拉曼光谱法检测中成药和保健品中添加的西地那非[J].药物分析杂志,2014,34(7):1241-1246.
[23]王琳,王雪,田静秒,等.表面增强拉曼光谱检测保健品中的盐酸吡咯列酮,盐酸罗格列酮与盐酸苯乙双胍[J].食品工业技术,2016,37(13):295-299.
[2]国家食品药品监督管理局.药品检验补充检验方法和检验项目批准件 2009030 补肾壮阳药物中成药中PDE5型抑制剂的快速检测方法[S].2009.
[3]国家食品药品监督管理局.国家食品补充检验方法 BJS201601食品中那非类物质的测定[S].2016.
[4]国家食品药品监督管理局.国家食品补充检验方法 BJS201704食品中去甲基他达拉非和硫代西地那非的测定高效液相色谱-串联质谱法[S].2017.
[5]国家食品药品监督管理局.国家食品补充检验方法 BJS201710 保健食品中75种非法添加化学药物的检测[S].2017.
[6]李绍辉,吴寒秋,许秀丽,等.超高效液相色谱串联质谱法检测玛咖产品中非法添加西地那非[J].食品工业科技,2016,37(11):310-313.
[7]陈聪,向平,沈保华,等.体液中西地那非的测定及其代谢物的确认[J].分析化学,2011,39(7):1093-1099.
[8]何涛,胡佳,张韬,等.壮阳作用药酒中枸橼酸西地那非非标研究[J].光明中医,2016,31(14):2039-2040.
[9]裘一婧,邹耀华.UPLC-Q-TOF-MS测定保健食品中非法添加的未知西地那非类物质[J].中国现代应用药学,2015,32(8):1000-1004.
[10]张健,丁涛,刘芸,吕辰,等.超高效液相色谱-串联质谱法测定保健品中9种非法添加的壮阳类化学药物[J].环境化学,2016,35(2):415-418.
[11]贾华,尹瑞林,钟旭,等.分子印迹复合膜对降糖药的拉曼光谱快速检测[J].高等学校化学学报,2016,37(2):239-245.
[12]顾振华,赵宇翔,吴卫平,等.表面增强拉曼光谱法快速检测水产品中的孔雀石绿[J].化学世界,2011,52(1):14-16.
[13]赵宇翔,彭少杰,赵建丰,等.表面增强拉曼光谱法快速检测牛奶中的三聚氰胺[J].乳业科学与技术,2011,34(1):27-29.
[14]杨宇,翟晨,彭彦昆,等.基于表面增强拉曼的饮料中山梨酸钾快速定量检测方法[J].光谱学与光谱分析,2017,37(11):3460-3464.
[15]黄双根,吴燕,胡建平,等.大白菜中马拉硫磷农药的表面增强拉曼光谱快速检测[J].农业工程学报,2016,32(6):296-301.
[16]陈文,朱莉娅,韩宇,等.表面增强拉曼光谱技术应用于西瓜中杀螟硫磷农药残留的检测[J].食品科技,2018,43(1):320-325.
[17]刘燕德,张宇翔,王海阳.脐橙表皮两种混合农药残留的表面增强拉曼光谱定量检测[J].光谱学与光谱分析,2018,38(1):123-127.
[18]王乐,张爱霞,陈晞,郑新华,等.表面增强拉曼光谱法快速检测饮料中玫瑰红B[J].食品研究与开发,2018,39(7):126-130.
[19]钟柳芳,何玲,陈钰婷.枸橼酸西地那非片近红外定性模型的建立[J].今日药学,2018,28(3):159-161.
[20]王学良,冯艳春,胡昌勤.近红外特征谱段相关系数法测定中药胶囊中添加枸橼酸西地那非[J].分析化学,2009,37(12):1825-1828.
[21]王红梅,李玲玲,陈海滨,等.表面增强拉曼光谱对西地那非类药物的快速检测[J].高等学校化学学报,2017,38(6):1040-1045.
[22]刘元瑞,葛海生,赵康虎,等.薄层原位表面增强拉曼光谱法检测中成药和保健品中添加的西地那非[J].药物分析杂志,2014,34(7):1241-1246.
[23]王琳,王雪,田静秒,等.表面增强拉曼光谱检测保健品中的盐酸吡咯列酮,盐酸罗格列酮与盐酸苯乙双胍[J].食品工业技术,2016,37(13):295-299.