珠江三角洲水域底泥中孔雀石绿、结晶紫及其代谢物分析

Analysis of malachite green and crystal violet and its metabolites in water sediment of Pearl River Delta

分析孔雀石绿(MG)、隐色孔雀石绿(LMG)、结晶紫(CV)、隐色结晶紫(LCV)标样的稳定特性(光、热),结果表明:LMG、LMG、CV和LCV在自然光下照射40 h,出现不同程度降解,降解率分别为21.6%,26.5%,18.19%,29.28%。四种标样在0—50℃避光处理2 h,均未出现明显降解。同时,采用高效液相色谱技术对珠江三角洲水产养殖池塘和珠江出海口底泥的MG、LMG、CV和LCV含量进行了分析。样品采用乙腈:二氯甲烷=1︰1萃取两次,经Pb O2柱后衍生后检测,检测方法回收率为76.3%—89.9%,RSD≤3.9%,检出限为0.001—0.0043μg·m L–1,结果表明:水产养殖池塘10个取样点的底泥均有MG残留,残留量最高的达0.0307μg·g–1,其它样品残留量在0.0011—0.0152μg·g–1之间;其中有3个取样点底泥有LMG残留,残留量在0.0073—0.0309μg·g–1之间。珠江河口的虎门、蕉门、鸡啼门、磨刀门、虎跳门和崖门均检测到CV,含量在0.0028—0.0361μg·g–1,洪沥门和横门均未检出CV。所有取样点均未检出到LCV。

The light, thermal and oxygen stability of malachite green（MG）, leuco malachitegreen（LMG）, crystal violet（CV） and leuco crystal violet（LCV） were studied in this paper. The results showed that LMG, CV, LCV put under natural light for 40 hours degraded by rates of 21.6%, 26.5%, 18.19%, 29.28% respectively. No distinct degradation was observed when these four samples were all put under 0-50 ℃without light. Meanwhile, high performance liquid chromatography（HPLC） technique was used to analyze the content of MG, LMG, CV, LCV in sediment sampling from some aquaculture ponds of Pearl River Delta and the Pearl River estuary. The samples were tested after extraction twice by acetonitrile, dichloromethane = 1：1 and derivative treatment by Pb O2 column. The recovery of this method were ranged from 76.3%-89.9%, with the relative standard deviation（RSD）of ≤3.9% and the limit detection of 0.001-0.0043 μg·m L–1. The results showed that there was MG residue in all 10 sampling sites of aquaculture ponds, with highest residual quantity of 0.0307 μg·g–1. The residual quantity in other sampling sites ranged from 0.001 to 0.0152 μg·g–1. LMG residue was detected in three of these 10 sampling sites, with quantity of 0.0073-0.0309 μg·g–1. CV residue was detected in Humen, Jiaomen, Jitimen, Modaomen, Hutiaomen and Yamen of Pearl River with quantity of 0.0028—0.0361μg·g–1. There was no CV residue detected in Henglimen and Hengmen. Also, no LCV residue was detected in all sampling sites.