Development of an automated on-line pre-column derivatization procedure for sensitive determination of histamine in food with high-performance liquid chromatography-fluorescence detection.
An improved sensitive method was developed and validated for the determination of histamine in food samples by using automated on-line pre-column derivatization coupled with high performance liquid chromatography and fluorescence detection (HPLC-FLD). o-Phthaldialdehyde (OPA) was adopted as derivatization reagent, and a "sandwich" (OPA+histamine+OPA) aspiration mode for the automated on-line pre-column derivatization was found to efficiently enhance the method sensitivity and precision. Histamine in food samples was efficiently extracted with a methanol-phosphate buffer solution (50:50, v/v) at 60 degrees C for 30 min, and purified with Waters Oasis MCX solid-phase extraction (SPE) cartridge. The limit of quantification for this method is 0.2 mg/kg, which is very sensitive for histamine determination. With the "sandwich" injection program, 3.7% of relative standard deviation (RSD) was achieved by five replicative determinations of a sample blank spiked with 0.25 mg/kg histamine standard. Histamine in food samples such as fumitory skipjack and mackerel was analyzed with relative recoveries over 95% at spiking level of 150 mg/kg, as well as canned tuna fish and cheese with relative recoveries up to 98% at spiking levels of 0.50 and 5.0 mg/kg, respectively. The proposed method was validated with a sample from the Food Analysis Performance Assessment Scheme (FAPAS) as a standard certified material; and the results (140+/-6 mg/kg) agreed well with the assigned value (139 mg/kg).
Peng
Jin-Feng
JF
Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China.
Fang
Ke-Teng
KT
Xie
Dong-Hua
DH
Ding
Bin
B
Yin
Ju-Yi
JY
Cui
Xiao-Mei
XM
Zhang
Ying
Y
Liu
Jing-Fu
JF
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D006632:Histamine / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D013050:Spectrometry, Fluorescence / Q000379:methods*
D006632:Histamine