Objective A method for the rapid determination of 7 mycotoxin contaminants in Liushenqu was established using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).
Methods An Waters ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm) column was used as the stationary phase at 30℃. Mobile phase was acetonitrile and 5 mmol · L-1 ammonium formate solution (contained 0.1% formic acid) with gradient elution at a flow rate of 0.4 mL·min-1. Mass spectrometry was performed by using an ESI source in a multiple reaction monitoring positive ion mode.
Results The method had a good specificity. The developed method provided a good linearity for the 7 mycotoxins with their respective linear rangers. The correlation (r) ranged from 0.9987 to 0.9995. The average recoveries ranged from 84.7% to 108.0% with relative standard deviation (RSDs) of 2.8% to 5.8% (n=6). Among 10 samples which were selected for analysis, aflatoxin B1 was detected from 2 samples at concentration of 1.24 μg·kg-1 and 2.35 μg·kg-1. Other mytocoxins were not detected.
Conclusion The determinantion method is rapid, simple, and has high recovery rate. It is applicable for quality detection of mycotoxins in Liushenqu.
1.王玉霞, 毛鑫, 王熠, 等.六神曲炮制历史沿革及现代研究[J]. 时珍国医国药, 2017, 28(5): 1182-1184. [Wang YX, Mao X, Wang Y, et al. The historical evolution and modern rsearch of Liushen Qu[J]. Lishizhen Medicine and Materia Medica Research, 2017, 28(5): 1182-1184.] DOI: 10.3969/j.issn.1008-0805.2017.05.060.
2.曹美娇, 张婷婷, 许枬, 等. NMR 法分析鉴定神曲的发酵产物[J]. 中国现代中药, 2017, 19(2): 183-187. [Cao MJ, Zhang TT, Xu D, et al. Identification of chemical component in SHEN QU based on NMR analysis[J]. Modern Chinese Medicine, 2017, 19(2): 183-187.] DOI: 10.13313/j.issn.1673-4890.2017.2.004.
3.仇雪, 任娟, 呼木吉勒图, 等. 市售六神曲质量研究[J]. 中南药学, 2019, 17(8): 1260-1263. [Qiu X, Ren J, Humu JLT, et al. Quality of Liushenqu in the market[J]. Central South Pharmacy, 2019, 17(8): 1260-1263.] DOI: 10.7539/j.issn.1672-2981.2019.08.017.
4.尹磊, 朱月健, 李冬梅, 等. 六神曲炮制及现代研究进展[J]. 亚太传统医药, 2021, 17(1): 186-189. [Yin L, Zhu YJ, Li DM, et al. Analysis of the process evolution and modern research progress of Massa Medicata Fermentata[J]. Asia-Pacific Traditional Medicine, 2021, 17(1): 186-189.] DOI: 10.11954/ytctyy.202101057.
5.张红玲, 孙佳彬, 覃艺, 等. 六神曲最佳发酵周期研究[J]. 亚太传统医药, 2018, 14(4): 31-34. [Zhang HL, Sun JB, Qin Y, et al. Investigation on the optimal fermentation period of Massa Medicata Fermentata[J]. Asia-Pacific Traditional Medicine, 2018, 14(4): 31-34.] DOI: 10.11954/ytctyy.201804012.
6.陈勇, 陈重均, 李劲, 等. 超高效液相串联质谱法检测三七药材中10种真菌毒素[J]. 药学学报, 2015, 50(1): 81-85. [Chen Y, Chen ZJ, Li J, et al. Determination of 10 mycotoxin contaminants in Panax notoginseng by ultra performance liquid chromatography-tandem mass spectrometry[J]. Acta Pharmaceutica Sinica, 2015, 50(1): 81-85.] DOI: 10.16438/j.0513-4870.2015.01.002.
7.刘文静, 黄彪, 傅建炜, 等. 超高效液相色谱-串联质谱法同时测定陈年老茶中16种真菌毒素残留[J]. 食品科学, 2021, 42(2): 299-305. [Li WJ, Huang B, Fu JW, et al. Simultaneous determination of 16 mycotoxin residues in aged tea by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food Science, 2021, 42(2): 299-305.] DOI: 10.7506/spkx1002-6630-20200611-157.
8.许莉, 黄晓婧, 罗霄, 等. 使君子中22种真菌毒素UHPLC-MS/MS同步检测与风险评估[J]. 时珍国医国药, 2021, 32(4) : 984-987. [Xu L, Huang XJ, Luo X, et al. Synchronous determination and risk evaluation of 22 mycotoxin contaminants in Shijunzi with UHPLC-MS/MS[J]. Lishizhen Medicine and Materia Medica Research, 2021, 32(4): 984-987.] DOI: 10.3969/j.issn.1008-0805. 2021.04.63.
9.中国药典2020年版. 一部[S]. 2020: 280-283.
10.国家卫生和计划生育委员会, 国家食品药品监督管理总局. 食品中真菌毒素限量: GB 2761—2017[S]. 2017: 2-5.
11.陈彦琳, 王云庭, 关凯乐, 等. 六神曲发酵过程中微生物群落结构研究[J]. 中国中药杂志, 2020, 45(21): 5219-5225. [Chen YL, Wang YT, Guan KL, et al. Investigation of microbial community involved in fermentation of Massa Medicata Fermentata[J]. China Journal of Chinese Materia Medica, 2020, 45(21): 5219-5225.] DOI: 10.19540/j.cnki.cjcmm.20200819.301.
12.韩凤, 李正刚, 刘丽. 高效液相色谱-荧光检测法同时测定六神曲(炒)中4种黄曲霉毒素[J]. 中国医药导刊, 2022, 24(11): 1138-1141. [Han F, Li ZG, Liu L. Simultaneous determination of four kinds of aflatoxin in massa medicate fermentata (fried) by HPLC-FLD[J]. Chinese Journal of Medicinal Guide, 2022, 24(11): 1138-1141.] DOI: 10.3969/j.issn.1009-0959.2022.11.020.
13.石柳. 淡豆豉和六神曲内外源污染物考察及主要活性物质分析[D]. 黑龙江省中医药科学院, 2022.
14.郑润生, 徐晖, 彭苑霞, 等. 稀释法结合LC-MS/MS检测在10种中药材污染黄曲霉毒素高通量筛查中的应用研究[J]. 中国中药杂志, 2014, 39(2): 273-277. [Zheng RS, Xu H, Peng YX, et al. A high throughput coupled with high performance liquid chromatography-tandem mass spectrometry method for determination of aflatoxin B1, B2. G1, G2 in 10 traditional Chinese medicines[J]. China Journal of Chinese Materia Medica, 2014, 39(2): 273-277.] DOI: 10.4268/cjcmm2014022.2.
15.罗朝权, 张敏玲, 郑润生, 等. 6种动物类药材中黄曲霉毒素污染的液质联用检测[J]. 中国实验方剂学杂志, 2018, 24(3) : 67-71. [Luo CQ, Zhang ML, Zheng RS, et al. Detection of aflatoxin contamination in 6 traditional Chinese animal medicines by LC-MS/MS[J]. Chinese Journal of Experimental Traditional Medical Formulae, 2018, 24(3): 67-71.] DOI: 10.13422/j.cnki.syfjx.201803006.7.
16.耿昭, 李小红, 苟琰, 等. QuEChERS法结合气相色谱-串联质谱法测定贝母类中药中53种农药残留[J]. 中草药, 2020, 51(20): 5337-5347. [Geng Z, Li XH, Gou Y, et al. Determination of 53 pesticide residues in different category of fritillaria by QuEChERS and GC-MS/MS[J]. Chinese Traditional and Herbal Drugs, 2020, 51(20): 5337-5347.] DOI: 10.7501/j.issn.0253-2670.2020. 20.028.