固相萃取-超高效液相色谱-串联质谱法测定母乳中三氯生和三氯卡班  

Determination of triclosan and triclocarban in human breast milk by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

作　　者：张品[1] 张晶[2] 石莹[3] 邵兵[2] 

机构地区：[1]首都医科大学公共卫生学院,北京100069 [2]北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京市预防医学研究中心 [3]北京市朝阳区卫生局卫生监督所

出　　处：《卫生研究》2015年第2期294-298,共5页Journal of Hygiene Research

基　　金：国家自然科学基金(No.21177014);“十二五”国家科技支撑计划课题(No.2012BAK17B16)

摘　　要：目的建立母乳中三氯生和三氯卡班超高效液相色谱-串联质谱(UPLCMS/MS)联用检测方法。方法母乳样品经β-葡萄糖醛酸酶/芳基硫酯复合酶酶解,乙腈提取后,C18固相萃取小柱富集净化,以甲醇和水作为液相色谱分析流动相,目标化合物经Waters ACQUITYTMUPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离后采用三重四极杆串联质谱仪负离子模式进行检测,同位素内标法定量。结果三氯生和三氯卡班分别在0.2~20.0μg/L与0.02~2.0μg/L范围内线性关系良好,相关系数(r2)均大于0.999,方法定量限分别为0.41和0.03μg/kg。3个水平的平均加标回收率为100.2%~119.3%,相对标准偏差为5.91%~11.31%(n=6)。利用该方法分析了25份母乳样品,均检出三氯生与三氯卡班,三氯生的浓度范围为<LOQ^0.77μg/kg,三氯卡班的浓度范围在<LOQ^4.28μg/kg。结论 UPLC-MS/MS法具有较高的灵敏度和重现性,可用于母乳中三氯生和三氯卡班的同时测定。Objective 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）. Methods 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^TM HSS T3 column（ 100 mm × 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. Results Satisfactory linearity（ r^2〉 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 from100. 2% to 119. 3%,with the relative standard deviations（ RSDs） between 5. 91% and11. 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.Conclusion Due to its high sensitivity and good reproductivity,this method can be applied to analyze TCS and TCC in human breast milk.

关 键 词：三氯生 三氯卡班 母乳 固相萃取 超高效液相色谱–串联质谱法 

分 类 号：R174[医药卫生—妇幼卫生保健] R155.51[医药卫生—公共卫生与预防医学]