欢迎登录材料期刊网

材料期刊网

高级检索

建立了保健酒中16种邻苯二甲酸酯类物质(PAEs)的气相色谱-三重四极杆质谱( GC-QQQ-MS)测定法。样品采用正己烷提取,使用 GC-QQQ-MS 测定,监测方式为选择离子监测( SIM),利用保留时间和碎片离子丰度比值判断定性结果,利用特征离子质量色谱峰峰面积-浓度标准曲线法定量,并用建立的方法分析了81批实际样品。实验结果表明:目标化合物特征离子质量色谱峰的峰面积与其质量浓度在各自的浓度范围内线性关系良好( r2≥0.9959)。在低、中、高3个浓度的添加水平下样品加标回收率除邻苯二甲酸二甲酯( DMP)为52.3%~58.7%外,其余15种化合物为88.6%~107.3%,相对标准偏差( RSD,n =6)为0.1%~6.8%。检出限为0.002~0.061 mg / L,定量限为0.005~0.202 mg / L。该方法具有灵敏、简单、准确、线性范围宽等优点,可满足保健酒中邻苯二甲酸酯类物质的检测需要。

A method for the analysis of sixteen phthalate acid ester( PAE)residues in health wine was developed using gas chromatography-triple quadrupole mass spectrometry(GC-QQQ-MS). The health wine samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The samples were detected by GC-QQQ-MS with electron impact source( EI) in selected ion monitoring( SIM)mode after extraction. The separation was performed on an HP-5MS capillary column( 30 m × 0. 25 mm × 0. 25 μm ) with temperature programming. The retention time and the fragment ion abundance ratio were used to judge the qualitative results, and the quantitation was performed with standard curve method of the characteristic ion chrom-atographic peak area-concentration. Eighty-one batches of health wine samples were detected using the method. The results showed that the method had good linear relationships with corre-lation coefficients(r2 )not less than 0. 995 9. The recoveries of fifteen PAEs ranged from 88. 6%to 107. 3% except dimethyl phthalate( DMP)which was 52. 3% -58. 7% in all the three spiked levels with the relative standard deviations of 0. 1% -6. 8%(RSD,n = 6). The limits of detection were between 0. 002 mg / L to 0. 061 mg / L. The limits of quantification were between 0. 005 mg / L and 0. 202 mg / L. The method is accurate,sensitive,proprietary and suitable for the sim-ultaneous determination of the sixteen phthalate acid esters in health wine.

参考文献

[1] 唐熙;李小晶;熊文明.[J].分析试验室,201332(02):31.
[2] 周相娟;赵玉琪;李伟.[J].日用化学工业,201040(02):148.
[3] 章勇;张蓓蓓;赵永刚.[J].分析试验室,201433(03):303.
[4] 塑化剂 .[OL].百度百科,2014-08-17.
[5] 吕建霞;李景林;胡永彪;等) .[OL].http://www.thermo.com.cn/Resources/201211/2315641328.pdf,2014-08-17.
[6] 黄晓东;陶然;徐强.[J].食品科学,201233(16):237.
[7] 白舟;李颢;谢佳.[J].湖北农业科学,201251(04):823.
[8] 肖佳;黄颖;王敏毅.[J].色谱,201230(09):951.
[9] 马燕玲;陈令新;丁养军.[J].色谱,201331(02):155.
[10] 杨荣静;卫碧文;高欢.[J].环境化学,201231(06):925.
[11] 李拥军;熊文明;陈坚文.[J].分析测试学报,201231(03):278.
[12] 袁永添;刘正华;李拥军.[J].广州农业科学,2012(06):100.
[13] 刘芃岩;高丽;申杰.[J].色谱,201028(05):517.
[14] 郑向华;林立毅;方恩华.[J].色谱,201230(01):27.
[15] 梁婧;庄婉娥;魏丹琦.[J].色谱,201230(03):273.
[16] 杨悠悠;谢云峰;田菲菲.[J].色谱,201331(07):674.
[17] 张莉;尚楚翔;孙成.[J].色谱,201432(06):653.
[18] GB/T 21911-2008.[S].
[19] GB 9685-2008.[S].
[20] 卫生部.卫生部办公厅关于通报食品及食品添加剂邻苯二甲酸酯类物质最大残留量的函(卫办监督函[2011]551 号[J].http://www foodmate net/law/shipin/175051 html,2014-08-17
上一张 下一张
上一张 下一张
计量
  • 下载量()
  • 访问量()
文章评分
  • 您的评分:
  • 1
    0%
  • 2
    0%
  • 3
    0%
  • 4
    0%
  • 5
    0%