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Objective To establish a method for simultaneous determination of 13 kinds of illegally added azo industrial dyes (Sudan red I, Sudan red II, Sudan red III, Sudan red IV, Sudan red B, rhodamine B, Sudan red G, Sudan red 7B, para red, Sudan orange G, basic orange 2, basic orange 21, and basic orange 22) in spices using ultra performance liquid chromatography tandem mass spectrometry. Methods After the sample was soaked with water, it was extracted with acidified acetonitrile (containing 1% acetic acid) by ultrasonic extraction, and purified with anhydrous magnesium sulfate and sodium chloride. After concentration, acetonitrile-0.10% formic acid aqueous solution was used as mobile phase, gradient elution, C18 chromatographic column (2.1 mm×150 mm, 1.7 µm) separation, electrospray multi reaction monitoring and positive ion mode determination were used to qualitatively determine 13 kinds of azo industrial dyes in spices, and external standard method was used for quantitative determination. Results The 13 kinds of azo industrial dyes showed good linear relationships within the mass concentration ranges of 0.5-50.0, 1-50, or 4-100 ng/mL, with correlation coefficients (r2) all greater than 0.99; the limits of detection could reach 1.0-10.0 µg/kg, and the limits of quantification could reach 3.0-30.0 µg/kg. The average spiked recovery rates at 1-fold, 2-fold, and 10 fold concentration levels were 75.7% to 102.4%, with relative standard deviations below 10% (n=6). Conclusion This method has the advantages of simple pretreatment, rapid, accurate, and sensitive, and is suitable for rapid screening and quantitative detection of 13 kinds of azo industrial dyes in spices, in order to provide strong technical support for the supervision of illegal addition of azo industrial dyes.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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