Shih T S, Chou J S, Chen C Y, Smith T J
Institute of Occupational Safety and Health, Council of Labor Affairs, Taipei, Taiwan, Republic of China.
Occup Environ Med. 1999 Jul;56(7):460-7. doi: 10.1136/oem.56.7.460.
To simplify the current preparation of samples, and to improve the specificity and reliability of the conventional analytical methods to measure urinary alkoxyacetic acids.
Samples containing alkoxyacetic acids including methoxy, ethoxy, and butoxyacetic acids (MAA, EAA, and BAA) were acidified with HCl and extracted with a mixed solvent of methylene chloride and isopropyl alcohol, then analysed by gas chromatography/mass spectrometry (GC/MS).
Optimal results were obtained when pH was 1.05-1.45, the ratio of methylene chloride and isopropyl alcohol was 2:1, and when extraction time was 10 minutes. Over the concentration range 0.3-200 micrograms/ml, MAA, EAA, and BAA could be determined with a pooled coefficient of variation (nine concentrations, six replicate samples) of 5.55%, 6.37%, and 6.41%, respectively. Urine samples were stable for at least 5 months and 3 freeze-thaw cycles at -20 degrees C. The limits of detection of MAA, EAA, and BAA were 0.055, 0.183, and 0.009 microgram/ml, respectively. The matrix effect of urine samples was negligible for MAA and EAA, but were marginally significant for BAA. The average recoveries of alkoxyacetic acids were 99%-101%. In urine samples MAA from 15 exposed workers showed a strong linear correlation (r = 0.999, slope = 1.01) between the new GC/MS method and Sakai's GC method.
The simplified non-derivatisation pretreatment of samples coupled with GC/MS can provide a specific, sensitive, simple, safe, and reliable method for the biological monitoring of occupational exposure of ethylene glycol ethers.
简化当前样品制备过程,提高常规分析方法测量尿中烷氧基乙酸的特异性和可靠性。
含有甲氧基、乙氧基和丁氧基乙酸(MAA、EAA和BAA)等烷氧基乙酸的样品用盐酸酸化,并用二氯甲烷和异丙醇的混合溶剂萃取,然后通过气相色谱/质谱联用仪(GC/MS)进行分析。
当pH为1.05 - 1.45、二氯甲烷与异丙醇的比例为2:1且萃取时间为10分钟时可获得最佳结果。在0.3 - 200微克/毫升的浓度范围内,MAA、EAA和BAA的合并变异系数(九个浓度,六个重复样品)分别为5.55%、6.37%和6.41%。尿液样品在-20℃下至少5个月和3次冻融循环保持稳定。MAA、EAA和BAA的检测限分别为0.055、0.183和0.009微克/毫升。尿液样品对MAA和EAA的基质效应可忽略不计,但对BAA有轻微显著影响。烷氧基乙酸的平均回收率为99% - 101%。在15名接触者的尿液样品中,新的GC/MS方法与Sakai的GC方法测得的MAA之间显示出强线性相关性(r = 0.999,斜率 = 1.01)。
样品简化的非衍生化预处理结合GC/MS可为乙二醇醚职业暴露的生物监测提供一种特异、灵敏、简单、安全且可靠的方法。