Microsoft Word 谢强胜二校出2087

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1 7 5 Vol. 7 No Journal of Food Safety and Quality May, A 谢强胜 1*, 谢春红 2, 刘春霖 1, 吴晓云 1, 贾廷辰 1, 李启艳 (1., ; 2., ) 1 摘要 : 目的 - A 方法, -, 结果 A 0.75~15 ng/ml (r=0.996), mg/kg %~96.4%, RSD 1.9%~5.6%(n=6), 0.06 μg/kg 0.20 μg/kg 结论, A 关键词 : - ; A; Determination of bisphenol A in fish oil soft capsules by ultra performance liquid chromatography tandem mass spectrometry XIE Qiang-Sheng 1*, XIE Chun-Hong 2, LIU Chun-Lin 1, WU Xiao-Yun 1, JIA Ting-Chen 1, LI Qi-Yan 1 (1. Shandong Institute for Food and Drug Control, Jinan , China; 2. Huangdao District Hospital, Qingdao , China) ABSTRACT: Objective To establish a method for the determination of bisphenol A(BPA) in fish oil soft capsules by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Method By optimizing extraction solvents and methods, BPA in fish oil soft capsules was extracted and then determined by UPLC-MS/MS using acetonitrile and water as mobile phase for gradient elution. And then mass-spectrography was performed with negative electrospray ionization mode and multiple reaction monitoring (MRM) mode. Results BPA had a good linear relationship in the range of 0.75~15 ng/ml with correlation coefficient of The recoveries at 3 levels of 1, 5, 10 mg/kg were 88.7%~96.4%, and the relative standard deviations (RSD) were 1.9%~5.6% (n=6), The limits of detection (LODs) and the limits of quantitation (LOQ) were 0.06 µg/kg and 0.20 μg/kg respectively. Conclusions The method is sensitive, specific and accurate, which is suitable for the determination of bisphenol A in fish oil soft capsules. KEY WORDS: ultra performance liquid chromatography-tandem mass spectrometry; bisphenol A; fish oil soft capsules 1 引言 A(bisphenol A, BPA),, [1] BPA, [3], * 通讯作者 :,,, xie_qsh@163.com *Corresponding author: XIE Qiang-Sheng, Associate Chief Pharmacist, Shandong Institute for Food and Drug Control, No.2749, Xinluo Avenue, Gaoxin District, Jinan , China. xie_qsh@163.com

20 μg/kg 结论, A 关键词 : - ; A; Determination of bisphenol A in fish oil soft capsules by ultra performance liquid chromatography tandem mass spectrometry XIE Qiang-Sheng 1*, XIE Chun-Hong 2, LIU

2 2088 7, BPA, [2-11], BPA [12],, [13],, BPA,, BPA, A [14,15], BPA BPA - - [16-18] - (ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS),,,, UPLC-MS/MS A, 2 材料与方法 2.1 材料,,, R, 2.2 仪器与试剂 (, Merck ), (, Merck ); A(Dr.Ehrenstorfer GmbH, : 11177, : 99.5%) Agilent ( ); MettlerToledo MS ( ); KQ-500DE ( ); QL-866 ( ) 2.3 实验方法样品提取 1 g ( 0.001g), 50 ml, 5 ml,, 5 ml, 3 min,,, 0.22 μm, UPLC-MS/MS 色谱条件 (1) : : Agilent Zorbax SB-C 18 (2.1 mm 50 mm, 1.8 μm); : A, B ; 1 ; 1 μl; 35 表 1 梯度洗脱程序 Table 1 Gradient elution program (min) A/% B/% 0~ ~ ~ ~ ~ (2) : : (electrospray ion mode, ESI - ), 20 psi; 200 ; 14 L/min; 250 ; 11 L/min; 3000 V, (multiple reaction monitoring, MRM) 2~3 Table 2 表 2 双酚 A 的质谱分析参数 MS parameters for the analysis of bisphenol A (m/z) (m/z) (ev) Table 3 表 3 质谱时间分段采集参数 Acquisition parameters of time subsection for mass spectrometry (min) 0 MRM To waste 2.5 MRM To MS 3.4 MRM To waste 标准曲线的绘制 A : A 10 mg, 100 ml,, A, A, ng/ml,, A (X) (Y) 3 结果与分析 3.1 质谱条件与色谱条件的选择质谱条件的优化,

001g), 50 ml, 5 ml,, 5 ml, 3 min,,, 0.22 μm, UPLC-MS/MS 2.3.2 色谱条件 (1) : : Agilent Zorbax SB-C 18 (2.1 mm 50 mm, 1.

3 第5期谢强胜, 等: 超高效液相色谱-串联质谱法测定鱼油软胶囊中的双酚 A 2089 量减小基质干扰, 提供高灵敏度和选择性的化合物分析模离子源模式下对 BPA 进行母离子扫描分析, 根据其相应强式考虑到流动相组成目标化合物的理化性质以及供试度和分子质量数, 确定为 ESI 负离子模式进行检测; 设定品溶液的特点, 选择离子化效率最佳的质谱条件因此, 选不同碰撞电压, 对选择的分子离子进行碰撞, 根据所获得择鞘气温度为 250, 鞘气流速为 11 L/min, 雾化气温度的质谱图中离子丰度, 确定和为 200, 雾化器流速为 14 L/min 根据色谱保留时间及为检测离子对, 优化碰撞电压分别为 30 和 35 ev, 双酚 A 峰宽带, 采用分时间段进行采集, 见表 3 通过在 ESI 正负的 MRM 色谱图见图 1, 供试品 MRM 色谱图见图 2 图 1 双酚 A 标准品的 MRM 色谱图 Fig. 1 MRM chromatograms of BPA 备注: 1 为总离子流图, 2 3 为提取离子流色谱图 1: TIC chromatogram, 2, 3: EIC chromatograms

4 MRM Fig. 2 MRM chromatograms of samples 1, 2 3 1: TIC chromatogram, 2, 3: EIC chromatograms

5 5, : - A A Fig. 3 The standard curve of BPA 色谱条件的选择 BPA Agilent zorbax SB-C 18 Acquity UPLC HSS T3 Cortecs UPLC C 18, Agilent zorbax SB-C 18, 0.1% 10 mmol/,,,, 3.2 提取方式的选择,,, ( 85%) 3.3 标准曲线和检出限 BPA 1 μl UPLC-MS/MS,, BPA 0.75~15 ng/ml, r=0.996, 3 BPA, 3 10 BPA 0.06 μg/kg 0.20 μg/kg 3.4 回收率及精密度实验 BPA, mg/kg, 6, 实际样品的检测 152 (2015 ), 11 BPA, 7.2%, 24~409 μg/kg A, A, 表 4 回收率及精密度结果 (n=6) Table 4 Results of precisions and recoveries (mg/kg) (%) RSD(%) 结论 - A,, μg/kg, 88.7%~96.4%, RSD 10%,, A, 参考文献 [1],,,. UPLC-MS/MS A[J]., 2015, 32(14): Li JQ, QiY, Li MH, et al. Determination of nonylphenol and bisphenol A in milk powder by UPLC-MS/MS [J]. Guangdong Chem Ind, 2015, 32(14):

5 实际样品的检测 152 (2015 ), 11 BPA, 7.2%, 24~409 μg/kg A, A, 表 4 回收率及精密度结果 (n=6) Table 4 Results of precisions and recoveries (mg/kg) (%) RSD(%) 1 88.7 5.6 5 92.5 4.2 10 96.4 1.

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Endocrine disrupting alkylphenols and bisphenol-a in coastal waters and supermaketseefood from Singapore [J]. Marine Pollut Bull, 2001, 48: 1145 1167. [5] Toyama Y, Suzuki-TouotaF, MaekawaM et al.

材料与方法仪器 ACQUITY UPLC Xevo TQ-S 三重四级杆液质联用仪 ( 美国 Waters 公司 ); 电喷雾离子源 (ESI), Masslynx 4.1 数据处理系统 (Waters);Thermo 低温离心机 ;KQ

材料与方法仪器 ACQUITY UPLC Xevo TQ-S 三重四级杆液质联用仪 ( 美国 Waters 公司 ); 电喷雾离子源 (ESI), Masslynx 4.1 数据处理系统 (Waters);Thermo 低温离心机 ;KQ [ 应用纪要 ] Rapid identification of 5 illegal additives in slimming health food by Xevo TQ-S 郝刚苏州市食品药品检验所, 苏州 15104 关键词超高效液相色谱 - 质谱, 多反应监测, 减肥类保健食品非法添加, 快速定性定量

Microsoft Word 谢强胜 二校 出2087

Microsoft Word 谢强胜二校出2087