5 9 Vol. 5 No. 9 2014 9 Journal of Food Safety and Quality Sep., 2014 吴 景 1, 陈 骁 鹏 2, 袁 华 峰 2, 曹 进 1*, 钱 忠 义 2, 邢 书 霞 1 (1., 100050; 2., 225300) 摘 要 : 目 的 方 法 (TLC), (HPLC), - (UPLC-MS) 结 果 ; 11.149 222.977 μg/ml, 结 论,,, 关 键 词 : ; ; ; ; - Determination of dioxopromethazine hydrochloride illegally adulteration in health care food WU Jing 1, CHEN Xiao-Peng 2, YUAN Hua-Feng 2, CAO Jin 1*, QIAN Zhong-Yi 2, XING Shu-Xia 1 (1. National Institutes for Food and Drug Control, Beijing 100050, China; 2. Taizhou Institute for Food and Drug Control, Taizhou 225300, China) ABSTRACT: Objective To establish a method for identification of dioxopromethazine hydrochloride illegally added in health care food. Methods The dioxopromethazine hydrochloride was identified by thin layer chromatography (TLC) and ultra performance liquid chromatography quadrupole time of flight mass spectrometry(uplc-qtof-ms), and the content was determined by high performance liquid chromatography (HPLC). Results The linear range of the method was between 11.149 and 222.977 μg/ml, and the regression equation was Y=4.8870 10 4 X+8.6351 10 3 with correlation coefficient of 0.9999. The detection limit was 1.115 μg/ml. Conclusion The method is convenient, reliable and accurate. It can be used to detect illegal adulteration of dioxopromethazine hydrochloride in health care food. KEY WORDS: health food; dioxopromethazine hydrochloride; illegally adulteration; high performance liquid chromatography; ultra performance liquid chromatography-quadrupole time of flight mass spectrometry 基 金 项 目 : (2013NC6) Fund: Supported by Youth Development Research Foundation of NIFDC (2013NC6) * 通 讯 作 者 :,,, E-mail: caojin@nifdc.org.cn *Corresponding author: CAO Jin, Associate Researcher, National Institutes of Food and Drug Control, No.2, Tiantan Xili, Dongcheng District, Beijing, 100050, China. E-mail: caojin@nifdc.org.cn
2664 5 1 引 言,,,,,,,,,, ; [1-3],,, TLC [4] HPLC [5-7] GC-MS [8] [9-11],, -,,,,, 2 仪 器 试 剂 与 材 料 Waters 2695-2996, DAD ( Waters ); Waters UPLC XEVO G2 QTOF ( Waters ); Mettler Toledo AL204 ( - ); KQ-700DE(700 W, 40 khz)( ) ( : 100299-201202, 99.9%, ),, ( : 0.5 g 60 ) 5 3 方 法 与 结 果 3.1 TLC 初 筛 0.5g,, 10 ml, 20 min,,, 1 mg/ml, ( 2010 Ⅵ B), 10 μl, GF 254, - - (65:45:1, v:v:v),,,, (254 nm),,, 1 1 Fig. 1 TLC chromatograms 1 3, 2 4 1 and 3: dioxopromethazine hydrochloride, 2 and 4: sample 3.2 液 相 色 谱 法 :, : 0.1% (v:v, 33:67) ; 226 nm; 190 400 nm; 1.0 ml/min; 35 105 2
9, : 2665, 0.2 mg/ml,, 50 ml,, 20 min,,,,, ;,, ; 10 μl,,, 2 3.3 超 高 效 液 相 - 质 谱 联 用 法 UPLC :, : 20 mmol/l (45: 55, v:v) ; 0.3 ml/min; 35 : (ESI), 3.0 kv, 120, 450, 800 L/h,,, 50 600 m/z 3.2,, 2 μl,, -, 3 3.4 线 性 关 系 考 察, 11.149 22.298 44.595 66.893 111.488 222.977 μg/ml, 10 μl,, (X), (Y),, Y=4.8870 10 4 X+8.6351 10 3, r=0.9999; 11.149 222.977 μg/ml 3.5 定 量 限 与 检 测 限 :, S/N 10, S/N 3, 0.5 g, 0.6 mg/g, 0.2 mg/g, 2 Fig. 2 HPLC chromatograms and UV spectrums A, B, C, D A and C: dioxopromethazine hydrochloride, B and D: sample
2666 5 3 Fig. 3 MS and MS 2 spectrum A, B A dioxopromethazine hydrochloride, B sample 3.6 稳 定 性 试 验 0 1 2 4 8 12 24 h, 10 μl, RSD 1.0% 24 h 3.7 加 样 回 收 实 验 6, 0.25 g,, 0.2230 g/ml 5 ml, 3.2, 3.2, 1, 99.80%, RSD 2.3%, 3.8 仪 器 精 密 度 实 验, 6,
9, : 2667 Table 1 表 1 盐 酸 二 氧 丙 嗪 回 收 率 实 验 结 果 Results of recoveries of dioxopromethazine hydrochloride (g) (mg) (mg) (mg) (recovery)/% (average recovery)/% RSD/% 0.2678 1.1971 1.115 2.2364 102.87 0.2468 1.1032 1.115 2.2103 99.28 0.2563 1.1457 1.115 2.2558 99.58 0.2592 1.1586 1.115 2.2540 98.31 99.80 2.3 0.2595 1.1600 1.115 2.2979 101.98 0.2576 1.1515 1.115 2.2292 96.76 10 μl,, RSD 0.6%, 3.9 系 统 适 用 性 考 察, : Waters Symmetry C 18 (4.6 mm 150 mm, 3.5 μm); Waters Sunfire C 18 (4.6 mm 250 mm, 5 μm); Agilent ZORBAX SB-C 18 (4.6 mm 150 mm, 3.5 μm), 3.2, 3, 3.10 样 品 中 盐 酸 二 氧 丙 嗪 的 筛 查 与 测 定 3.2 3.3,,,, 2 3 6 3.2,, 5, 2 4 讨 论 4.1 样 品 前 处 理,,, 4.2 方 法 的 选 择, TLC HPLC, TLC 表 2 样 品 中 盐 酸 二 氧 丙 嗪 的 含 量 测 定 结 果 Table 2 Content determination of dioxopromethazine hydrochloride in samples (mg/g) 20130102 4.47 20131209 ND L140602 ND 20131201 ND 140306 ND 20130323 ND : ND-, HPLC, UPLC-TOF-MS,, 3, 4.3 保 健 食 品 非 法 添 加 检 测 技 术 的 发 展 前 景,,,,,, [12-20],,,
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