食品研究与开发
食品研究與開髮
식품연구여개발
FOOD RESEARCH AND CEVELOPMENT
2015年
16期
128-131
,共4页
基质固相分散萃取%高效液相色谱%孔雀石绿%结晶紫
基質固相分散萃取%高效液相色譜%孔雀石綠%結晶紫
기질고상분산췌취%고효액상색보%공작석록%결정자
matrix solid-Phase dispersion(MSPD)%high performance liquid chromatography (HPLC)%mala-chite green(MG)%crystal violet (CV)
建立了基质固相分散-液相色谱法快速测定水产品中的孔雀石绿和结晶紫的新方法。将鱼肉样品粉碎后与C 18填料研磨混合，装柱、淋洗，洗脱液浓缩后用高效液相色谱检测。色谱条件：色谱柱Inertsil ODS-SP（5μm，4.6 mm×150 mm），乙腈和乙酸铵缓冲溶液体积比80∶20作流动相等度洗脱，流速1.00 mL/min，检测波长254 nm。结果表明，孔雀石绿和结晶紫在0.30μg/L~30.00μg/L范围内，线性关系良好，相关系数（r）均大于0.999，检测限（S/N=3）分别为：0.18 ng/g和1.10 ng/g，样品加标回收率分别为86.28%~98.79%和82.51%~93.71%，其精密度RSD均小于5%（n=5）。
建立瞭基質固相分散-液相色譜法快速測定水產品中的孔雀石綠和結晶紫的新方法。將魚肉樣品粉碎後與C 18填料研磨混閤，裝柱、淋洗，洗脫液濃縮後用高效液相色譜檢測。色譜條件：色譜柱Inertsil ODS-SP（5μm，4.6 mm×150 mm），乙腈和乙痠銨緩遲溶液體積比80∶20作流動相等度洗脫，流速1.00 mL/min，檢測波長254 nm。結果錶明，孔雀石綠和結晶紫在0.30μg/L~30.00μg/L範圍內，線性關繫良好，相關繫數（r）均大于0.999，檢測限（S/N=3）分彆為：0.18 ng/g和1.10 ng/g，樣品加標迴收率分彆為86.28%~98.79%和82.51%~93.71%，其精密度RSD均小于5%（n=5）。
건립료기질고상분산-액상색보법쾌속측정수산품중적공작석록화결정자적신방법。장어육양품분쇄후여C 18전료연마혼합，장주、림세，세탈액농축후용고효액상색보검측。색보조건：색보주Inertsil ODS-SP（5μm，4.6 mm×150 mm），을정화을산안완충용액체적비80∶20작류동상등도세탈，류속1.00 mL/min，검측파장254 nm。결과표명，공작석록화결정자재0.30μg/L~30.00μg/L범위내，선성관계량호，상관계수（r）균대우0.999，검측한（S/N=3）분별위：0.18 ng/g화1.10 ng/g，양품가표회수솔분별위86.28%~98.79%화82.51%~93.71%，기정밀도RSD균소우5%（n=5）。
A method for the determination of malachite green and crystal viole in aquatic products based on matrix solid-phase dispersion with liquid chromatography was established. Fish samples mix with C 18 after grinding, and then the blended material was transferred to a 6 mL SPE column. And then, the column was eluted with hexane, ethyl acetate and acetonitrile in sequential order. The eluent was collected and evaporated to dryness. The concentrated sample solution were filtrated with filter membrane(0.22μm),and then injected in to the HPLC system. The separation was carried on the inertsil ODS-SP (5 μm, 4.6 mm × 150 mm) chromatographic column with ammonium acetate/acetonitrile (80∶20) as mobile phase isocratic elution, and flow rate of 1.00 mL/min and the detection wavelength was 254 nm. The results show that, A good linearity (r>0.999) was achieved for the target compound over the range of 0.30μg/mL-30.00μg/mL. the limit of detection (S/N=3) of Calachite Green and Crystal Violer were 0.18 ng/g and 1.10 ng/g. the recoveries of Malachite Green and Crystal Violet from fish tissue ranged from 86.28%-98.79%and 82.51%-93.71%both with the relative standard deviations (RSD) within 5%.
