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1 5 9 Vol. 5 No 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., ; 2., ) 摘要 : 目的方法 (TLC), (HPLC), - (UPLC-MS) 结果 ; 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 , China; 2. Taizhou Institute for Food and Drug Control, Taizhou , 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 and μg/ml, and the regression equation was Y= X with correlation coefficient of The detection limit was 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 :,,, caojin@nifdc.org.cn *Corresponding author: CAO Jin, Associate Researcher, National Institutes of Food and Drug Control, No.2, Tiantan Xili, Dongcheng District, Beijing, , China. caojin@nifdc.org.cn

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 引言,,,,,,,,,, ; [1-3],,, TLC [4] HPLC [5-7] GC-MS [8] [9-11],, -,,,,, 2 仪器试剂与材料 Waters , DAD ( Waters ); Waters UPLC XEVO G2 QTOF ( Waters ); Mettler Toledo AL204 ( - ); KQ-700DE(700 W, 40 khz)( ) ( : , 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, and 3: dioxopromethazine hydrochloride, 2 and 4: sample 3.2 液相色谱法 :, : 0.1% (v:v, 33:67) ; 226 nm; nm; 1.0 ml/min;

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.

3 9, : 2665, 0.2 mg/ml,, 50 ml,, 20 min,,,,, ;,, ; 10 μl,,, 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,,, m/z 3.2,, 2 μl,, -, 线性关系考察, μg/ml, 10 μl,, (X), (Y),, Y= X , r=0.9999; 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

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.

4 Fig. 3 MS and MS 2 spectrum A, B A dioxopromethazine hydrochloride, B sample 3.6 稳定性试验 h, 10 μl, RSD 1.0% 24 h 3.7 加样回收实验 6, 0.25 g,, g/ml 5 ml, 3.2, 3.2, 1, 99.80%, RSD 2.3%, 3.8 仪器精密度实验, 6,

5 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/% 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 ,,,, ,, 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) ND L ND ND ND 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],,,

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.

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Chin J Anal Chem, 2009, 37( 11) : 1583 [18], 姮,. - [J]., 2010, 30(10) : 1913 Lu Y, Qiu YH, Liu JJ, et al.

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