建立了柱前衍生化-萃取阻断反应-高效液相色谱(HPLC)测定化妆品中甲醛的方法.化妆品中甲醛检测的难点是:甲醛缓释剂类防腐剂在衍生过程中释放甲醛,影响游离甲醛的准确测定.以2,4-二硝基苯肼(DNPH)乙腈溶液-磷酸盐缓冲液(pH2)(1∶1,v/v)为提取溶液,于室温下快速衍生2 min后,立即加入二氯甲烷萃取,阻断衍生反应,经乙腈稀释后进行HPLC测定.以Agilent C18柱(250 mm ×4.6 mm,5μm)为分离柱,乙腈-水(60∶40,v/v)为流动相,流速为1.0 mL/min,于355 nm波长下检测.在洗发水、乳液、膏霜、洗手液、牙膏、指甲油、粉饼中分别添加50、100、500、1 000 μg/g 4个浓度水平的甲醛,其回收率为81％～ 106％,相对标准偏差(n=6)＜5.0％.方法的定量限(以信噪比(S/N)＞ 10计)为50 μg/g.该方法快速、简便、重现性好,且可以有效避免甲醛缓释剂类防腐剂分解释放甲醛,适用于化妆品中游离甲醛的测定.
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