超高效液相色谱-串联质谱法快速测定蔬菜中4种异噻唑啉酮类化合物的含量

提出了超高效液相色谱-串联质谱法(UHPLC-MS/MS)快速测定蔬菜中5-氯-2-甲基-4-异噻唑啉-3-酮(CMIT)、2-甲基-4-异噻唑啉-3-酮(MIT)、1,2-苯并异噻唑啉-3-酮(BIT)、2-正辛基-4-异噻唑啉-3-酮(OIT)等4种异噻唑啉酮类化合物含量的方法。取10.0 g已匀浆的蔬菜样品,用10 mL乙腈超声提取30 min,离心,残渣重复提取一次,合并提取液,加入5 g氯化钠,振荡、静置后,于40℃氮吹至近干,用2 mL 10%(体积分数,下同)甲醇溶液溶解残渣。所得溶液过已活化的HLB固相萃取小柱,用5 mL 10%甲醇溶液淋洗,6 mL甲醇洗脱。洗脱液于40℃氮吹至近干后,用甲醇定容至1 mL,过0.22μm有机滤膜,滤液在ACQIUTY UPLC BEH SHIELD RP18色谱柱上分离,以不同体积比的甲醇-水混合液为流动相进行梯度洗脱,质谱分析采用多反应监测采集模式,电喷雾正离子扫描模式,基质匹配法绘制工作曲线。结果表明,4种异噻唑啉酮类化合物的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限(3S/N)分别为0.5,0.5,0.5,0.025...     

Determination of 14 whitening active components in cosmetics by ultra-high performance liquid chromatography-triple quadrupole mass spectrometryEI北大核心CSCD

A method based on ultra high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/ MS) was developed for the analysis of 14 whitening active components in oilycosmetics. The 14 whitening active components were extracted from cosmetics by supersonic extraction with 20 mmol / L potassium dihydrogen phosphate solution, purified by HLB solid phase extraction column and filtered with 0. 22 μm filter membrane. Shim-pack GIST C18 AQ chromatographic column was used for the separation of the whitening active components. Methanol-0. 1% formic acid solution(containing 5 mmol / L ammonium acetate)was employed as mobile phase for gradient elution, and the analytes were detected by electrospray ionization source with positive and negative ion alternate scanning mode and multiple reaction monitoring mode (MRM). The results showed that an effective separation was achieved within 10 min under the optimized conditions, 14 whitening active components exhibited good linear relationships in the respective linear range with the correlation coefficient more than 0. 999. The limits of detection were in the range of 0. 15-2. 5 mg / kg, and the limits of quantitation were in the range of 0. 5-7. 5 mg / kg. The recoveries were from 70% to 117%, and the relative standard deviations were between 0. 2% and 12% . © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

低共熔溶剂液-液微萃取/高效液相色谱法检测饮料和糖果中10种水溶性色素EI北大核心CSCD

以不同氢键供体和氢键受体合成的10种疏水型低共熔溶剂(DES)作为溶剂提取食品中合成色素,辅助液-液微萃取前处理技术,建立同时测定10种水溶性色素的高效液相色谱方法。结果表明:由四丁基氯化铵和辛酸合成的低共熔溶剂提取色素的效果最好,在最佳萃取条件(含水量0,摩尔比1∶3,提取剂用量500μL,提取温度20℃、振摇时间20 min)下,色素的回收率达83.5%~119.8%,仪器检出限为11.3~500.0μg/L。应用建立的方法测定汽水和糖果中的色素,赤藓红加标回收率在40%左右,其余色素加标回收率在77.8%~102.7%之间,相对标准偏差小于5.3%。