Zhang Pin, Zhang Jing, Shi Ying, Shao Bing
Wei Sheng Yan Jiu. 2015 Mar;44(2):294-8.
An analytical method was developed to simultaneously detect triclosan (TCS) and triclocarban (TCC) in human breast milk using solid-phase extraction (SPE) with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
Samples were extracted by acetonitrile and purified with C -18 SPE cartridge after enzymolysis with β-glucuronidase/arylsulfatase. The chromatographic separation was performed on a Waters ACQUITY UPLC™ HSS T3 column (100 mm x 2. 1 mm, 1. 8 µm) with gradient elution using methanol and water at a flow rate of 0. 3 ml/min. The target analytes were assayed by triple quadrupole mass spectrometer operating in the negative ion mode. Quantification was performed by isotopic internal standard calibration.
Satisfactory linearity (r2 > 0. 999) was obtained over the range of 0. 2 - 20. 0 µg/L and 0. 02 - 2. 0 µg/L for triclosan and triclocarban, respectively, with the limits of quantifications (LOQs) of 0. 41 and 0. 03 µg/kg. Average recoveries of two target compounds (spiked at three concentration levels) ranged from 100. 2% to 119. 3%, with the relative standard deviations (RSDs) between 5. 91% and 11. 31% (n =6). Twenty-five real samples (n = 25) were detected containing TCS and TCC at concentrations of < LOQ - 0. 77 µg/kg and < LOQ - 4. 28 µg/kg, respectively.
Due to its high sensitivity and good reproductivity, this method can be applied to analyze TCS and TCC in human breast milk.
建立一种采用固相萃取(SPE)结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测人母乳中三氯生(TCS)和三氯卡班(TCC)的分析方法。
样品经乙腈提取,用β-葡萄糖醛酸酶/芳基硫酸酯酶酶解后,通过C-18固相萃取柱进行纯化。采用Waters ACQUITY UPLC™ HSS T3柱(100 mm×2.1 mm,1.8 µm)进行色谱分离,以甲醇和水为流动相进行梯度洗脱,流速为0.3 ml/min。目标分析物采用在负离子模式下运行的三重四极杆质谱仪进行测定。通过同位素内标校准进行定量分析。
三氯生和三氯卡班在0.2 - 20.0 µg/L和0.02 - 2.0 µg/L范围内分别获得了令人满意的线性关系(r2>0.999),定量限(LOQ)分别为0.41和0.03 µg/kg。两种目标化合物(在三个浓度水平加标)的平均回收率在100.2%至119.3%之间,相对标准偏差(RSD)在5.91%至11.31%之间(n = 6)。检测了25份实际样品(n = 25),其中三氯生和三氯卡班的浓度分别为<LOQ - 0.77 µg/kg和<LOQ - 4.28 µg/kg。
该方法具有高灵敏度和良好的重现性,可用于分析人母乳中的三氯生和三氯卡班。