Determination of Total Sulfur Dioxide in Chinese Herbal Medicines via Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry
WANG Xiao-wei1, LIU Jing-fu2, GUAN Hong3, WANG Xiao-yan1, SHAO Bing1*, ZHANG Jing1, LIU Li-ping1, ZHANG Ni-na1
1. Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Centers for Diseases Control and Prevention & Centers for Preventive Medical Research, Beijing 100013, China 2. State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China 3. Shunyi District Centers for Diseases Control and Prevention, Beijing 101300, China
Abstract：As an important treatment method, sulfur fumigation plays an essential role in the production and preservation of traditional Chinese herbal medicines. Although there is strict regulation on the use of sulfur dioxide, the abuse of sulfur dioxide still occurred from time to time. And the public faces a high risk of exposure. Because of the poor precision and tedious preparation procedures of traditional recommended titration, the accurate and convenient determination of sulfur dioxide in Chinese herbal medicines is still a critical analytical task for medicines safety and the public health. In this study, an accurate, high-throughput, and convenient method for the absolute determination of SO2 in Chinese herbal medicines based on triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS/MS) technique is developed. The study compared the quantitative ability for sulfur when the ICP-MS operated under traditional single quadrupole (QMS) mode and novel triple quadrupole (MS/MS) mode with three Reaction/Collision cell condition (no gas, helium, and oxygen). The result indicated that when the concentration of sulfate ranging from 0.5 to 100 mg·L-1, isotopic 34S can be selected as quantitative ion either the ICP-MS operated under the QMS mode or MS/MS mode. The use of helium in the Reaction/Collision cell decreased the single intensity of background ions. Better than QMS mode, the MS/MS mode can effectively reduced background interference. But there are no significant differences about the linear range and limit of detection. However, when the ICP-MS operated under MS/MS mode and oxygen was used as reaction gas in the Reaction/Collision cell, the ICP-MS/MS provided an interference-free performance, the linear range and limit of detection improved significantly. Either 32S or 34S exhibits an excellent linearity (r>0.999) over the concentration range of 0.02～100 mg·L-1, with a limit of detection of 5.48 and 9.76 μg·L-1 for 32S16O2-4 and 34S16O2-4, respectively. The Chinese herbal medicines was treated using microwave digestion added 6 mL nitric acid and 2 mL hydrogen peroxide before analysis. The amount of nitric acid and hydrogen peroxide were optimized. The method was validated using Chinese herbal standard reference material GBW10020. The sample was treated and detected in six parallel, and the average concentrations obtained using the developed method (0.42%±0.01%) is in excellent agreement with the standard concentration (0.41%±0.03%). The study demonstrates an accurate and convenient approach for the quantification of SO2 in Chinese herbal medicines.
王晓伟1，刘景富2，关 红3，王小艳1，邵 兵1*，张 晶1，刘丽萍1，张妮娜1 . 三重串联四极杆电感耦合等离子体质谱法测定植源性中药材中总硫含量 [J]. 光谱学与光谱分析, 2016, 36(02): 527-531.
WANG Xiao-wei1, LIU Jing-fu2, GUAN Hong3, WANG Xiao-yan1, SHAO Bing1*, ZHANG Jing1, LIU Li-ping1, ZHANG Ni-na1. Determination of Total Sulfur Dioxide in Chinese Herbal Medicines via Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2016, 36(02): 527-531.
[1] Wang S, Cui X, Fang G. Food Chem., 2007, 103(4): 1487. [2] http://www.chp.org.cn/cms/newscenter/news/000502.html, 2013. [3] http://apps.who.int/iris/bitstream/10665/77763/1/9789241660679_eng.pdf?ua=1, 2012. [4] Sullivan J J, Hollingworth T A, Wekell M M, et al. J. Assoc Off Anal. Chem., 1990, 73(1): 35. [5] Bak F, Schuhmann A, Jansen K H. FEMS Microbiol. Ecol., 1993, 12(4): 257. [6] Aberl A, Coelhan M. Food Addit. Contam. Part A Chem. Anal. Control. Expo. Risk Assess, 2013, 30(2): 226. [7] Fang Y, Qian M C. J. Chromatogr A, 2005, 1080(2): 177. [8] Alberto N, Araújo Cristina M C M Couto, José L F C Lina, et al. J. AGR Food Chem., 1998, 46(1): 168. [9] Huang M, Becker-Ross H, Florek S, et al. Anal. Bioanal. Chem., 2005, 382(8): 1877. [10] Persson D P, Hansen T H, Laursen K H, et al. Metallomics, 2009, 1(5): 418. [11] Boulyga S, Heilmann J, Heumann K. Anal. Bioanal. Chem., 2005, 382(8): 1808. [12] Heilmann J, Boulyga S, Heumann K. Anal. Bioanal. Chem., 2004, 380(2): 190. [13] Weir A, Westerhoff P, Fabricius L, et al. Environ. Sci. Technol., 2012, 46(4): 2242. [14] http://www.chp.org.cn/export/sites/chp/resource/bio/2014032815280651580.pdf, 2013. [15] Gunduz S, Akman S. LWT-Food Sci. Technol., 2014, 59(2): 718. [16] Balcaen L, Woods G, Resano M, et al. J. Anal. At. Spectrom., 2013, 28: 33. [17] Fernández S D, Sugishama N, Encinar J R, et al. Anal. Chem., 2012, 84(14): 5851.
