CAJ | 학술논문

建立了三文鱼中孔雀石绿和无色孔雀石绿的同位素稀释质谱测定法,即:通过添加作为同位素稀释剂的氘代孔雀石绿和无色孔雀石绿到样品中,经液液萃取、提取中添加中性氧化铝以及过碱性氧化铝小柱进行净化的前处理,然后由以乙腈和乙酸铵缓冲液(0.05 mol/L, pH 4.5)为流动相的液相色谱/离子阱质谱联用来作为分离检测手段.对含不同浓度孔雀石绿和无色孔雀石绿的储备液在不同溶剂、酸度、时间和温度的稳定性,前处理过程中的中性氧化铝的合适添加量、破乳剂的选择、孔雀石绿和无色孔雀石绿在氮吹和旋蒸过程中的损失以及液相色谱和质谱条件进行了研究.该方法的孔雀石绿和无色孔雀石绿的回收率分别为95.6%～103.3%和97.64%～100.80%,检测限为0.4和0.3μg/kg,相对标准偏差分别为4.76%～6.13%和3.14%～5.67%.结果表明,所建立的方法快速、灵敏、准确、可靠.
건립료삼문어중공작석록화무색공작석록적동위소희석질보측정법,즉:통과첨가작위동위소희석제적도대공작석록화무색공작석록도양품중,경액액췌취、제취중첨가중성양화려이급과감성양화려소주진행정화적전처리,연후유이을정화을산안완충액(0.05 mol/L, pH 4.5)위류동상적액상색보/리자정질보련용래작위분리검측수단.대함불동농도공작석록화무색공작석록적저비액재불동용제、산도、시간화온도적은정성,전처리과정중적중성양화려적합괄첨가량、파유제적선택、공작석록화무색공작석록재담취화선증과정중적손실이급액상색보화질보조건진행료연구.해방법적공작석록화무색공작석록적회수솔분별위95.6%～103.3%화97.64%～100.80%,검측한위0.4화0.3μg/kg,상대표준편차분별위4.76%～6.13%화3.14%～5.67%.결과표명,소건립적방법쾌속、령민、준학、가고.
A quantitative liquid chromatography–-tandem mass spectrometric (LC–-MS/MS) method has been developed for the determination of malachite green (MG) and its metabolite leucomalachite green (LMG) in salmon fish. Residues were extracted with the acetonitrile–acetate system. The samples were purified by using neutral alumina in extraction process and alkaline alumina SPE column, then it was analyzed with a reversed-phase LC–MS/MS using a positive-ion electrospray ionisation (ESI). Isotope-labelled malachite green (MG-D5) and leucomalachite green (LMG-D5) were used as an internal standard for the quantification of MG and LMG residues. The detection limit for MG and LMG was 0.4 and 0.3 μg/kg, respectively. The relative recovery was in the range of 95.6%～103.3% for MG and 97.64%～100.80% for LMG. The stability of MG and LMG stock solutions was studied in different conditions, such as solvent, acidity, time and temperature. The loss of MG and LMG in the process of nitrogen blowing and vacuum evaporation was investigated.