RESUMO
OBJECTIVE:To establish the method for the determination of 9 illegal dyes in Carthamus tinctorius.METHODS:HPLC-MS/MS was adopted.The determination was performed on SB-C18 column with mobile phase consisted of 10 mmol/L ammonium formate-acetonitrile (gradient elution) at the flow rate of 0.2 mL/min.The column temperature was 30 ℃,and the sample size was 10 μL.Mass spectrometry condition:electrospray ion source,negative ion multi-ion reaction monitoring mode,ion spray voltage of 3 500 V,drying gas temperature of 350 ℃,drying gas flow rate of 10 L/min,colliding gas of high pure nitrogen gas,scanning range of m/z 50～ 1 000.RESULTS:The linear ranges of ponceau,acid red 73,lemon yellow,azorubin,allura red,gold orange Ⅱ,sunset yellow,pyrosine and golden orange G were 5.313 5～531.35 ng/mL(r=0.987 0),1.312 0～1 312.00 ng/mL(r=0.994 8),124.480 0～2 824.00 ng/mL(r=0.983 2),6.300 0～630.00 ng/mL(r=0.964 8),1.035 8～517.92 ng/mL(r=0.996 4),0.552 0～1 104.00 ng/mL(r=0.909 0),5.046 3～2 018.52 ng/mL(r=0.996 2),5.046 3～2 018.52 ng/mL(r=0.997 6),1.079 5～2 159.00 ng/mL(r=0.990 0),respectively.The limits of quantitation were 10.418 7,1.131 0,68.401 0,13.695 7,1.670 7,0.238 0,3.973 3,1.064 7,1.285 0 ng/kg.The limits of detection were 3.125 6,0.339 3,20.520 3,4.108 7,0.501 2,0.071 4,1.192 0,0.319 4,0.385 5 ng/kg,respectively.RSDs of precision,stability and reproducibility tests were all lower than 3.0％.The recoveries were 91.2％-99.1％ (RSD=0.7％-2.2％,n=6).CONCLUSIONS:The established method is specific,sensitive,simple and rapid,and can be used for the detection of 9 illegal dyes in C.tinctorius.
RESUMO
Objective To establish a thin layer chromatography-surface-enhanced Raman scattering(TLC-SERS) method for the detection of dyed Croci Stigma.Method The dyed Croci Stigma was wetted by ethanol and pressed on TLC plate sprayed with Silver sol.The pressed zone was immediately detected by a portable Raman spectrometer.Factors including the concentration of ethanol, spraying time and amount of silver sol were investigated and optimized.Results The dyed Croci Stigma, stained by auramine O, new fuchsin, tartrazine and brilliant ponceau were successfully detected using the established method.Conclusion The combination of TLC and SERS technology provides a rapid, simple and sensitive detection method which is suitable for quick field tests.
RESUMO
OBJECTIVE:To establish the method for the determination of 9 illegal dyes in Carthamus tinctorius.METHODS:HPLC-MS/MS was adopted.The determination was performed on SB-C18 column with mobile phase consisted of 10 mmol/L ammonium formate-acetonitrile (gradient elution) at the flow rate of 0.2 mL/min.The column temperature was 30 ℃,and the sample size was 10 μL.Mass spectrometry condition:electrospray ion source,negative ion multi-ion reaction monitoring mode,ion spray voltage of 3 500 V,drying gas temperature of 350 ℃,drying gas flow rate of 10 L/min,colliding gas of high pure nitrogen gas,scanning range of m/z 50～ 1 000.RESULTS:The linear ranges of ponceau,acid red 73,lemon yellow,azorubin,allura red,gold orange Ⅱ,sunset yellow,pyrosine and golden orange G were 5.313 5～531.35 ng/mL(r=0.987 0),1.312 0～1 312.00 ng/mL(r=0.994 8),124.480 0～2 824.00 ng/mL(r=0.983 2),6.300 0～630.00 ng/mL(r=0.964 8),1.035 8～517.92 ng/mL(r=0.996 4),0.552 0～1 104.00 ng/mL(r=0.909 0),5.046 3～2 018.52 ng/mL(r=0.996 2),5.046 3～2 018.52 ng/mL(r=0.997 6),1.079 5～2 159.00 ng/mL(r=0.990 0),respectively.The limits of quantitation were 10.418 7,1.131 0,68.401 0,13.695 7,1.670 7,0.238 0,3.973 3,1.064 7,1.285 0 ng/kg.The limits of detection were 3.125 6,0.339 3,20.520 3,4.108 7,0.501 2,0.071 4,1.192 0,0.319 4,0.385 5 ng/kg,respectively.RSDs of precision,stability and reproducibility tests were all lower than 3.0％.The recoveries were 91.2％-99.1％ (RSD=0.7％-2.2％,n=6).CONCLUSIONS:The established method is specific,sensitive,simple and rapid,and can be used for the detection of 9 illegal dyes in C.tinctorius.