Simultaneous Determination of 9 Illegal Dyes in Carthamus tinctorius by HPLC-MS/MS / 中国药房

ABSTRACT

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.