羊毛中大蒜素长效驱避剂检测方法建立及其缓释性能研究

Establishment of the detection method for allicin long-acting tick repellent and its evaluation of slow release performance

研究A、B、C 3个配方的大蒜素长效驱避剂的缓释性能及其与普通大蒜素水乳液的差异。建立羊毛中大蒜素的气相色谱检测方法,对影响羊毛中大蒜素检出的萃取时间、萃取液体积、萃取温度及羊毛浸泡时间进行单因素试验条件优化与筛选,采用所建立方法对浸泡过相应驱蜱剂的羊毛分别于0 d、1 d、2 d、3 d、5 d、8 d、12 d、18 d检测其大蒜素含量,并以第0天羊毛中所测得的大蒜素含量为初始值,其他各时间点为余留值,得到不同配方的大蒜素的相对释放率,绘制时间/相对释放率曲线,结合不同处理组同一时间点的大蒜素含量进行差异性分析,对3个大蒜素驱避剂的缓释性能进行评价。结果供试羊毛在大蒜素水乳液中浸泡15 min,3 mL无水乙醇中35℃萃取15 min,所测得的萃取液中大蒜素峰面积最大,利于其定量检测。对3组不同配方大蒜素长效驱避剂的缓释性能测定中,A组在1 d、2 d、3 d、5 d时,每克羊毛中大蒜素含量分别为(4 181.93±201.89)μg、(2 317.84±113.12)μg、(1 662.96±96.03)μg、(1 037.51±32.07)μg,显著高于其他处理组,其大蒜素相对释放率分别为31.3%、61.9%、72.7%、82.9%;B组在1 d、2 d、5 d时,每克羊毛中大蒜素含量分别为(3 324.70±194.78)μg、(1 691.17±131.46)μg、(764.03±46.75)μg,高于C组和对照组,且差异显著(P<0.05),相对释放率分别为46.6%、72.9%、87.7%;C组在1 d、2 d时,每克羊毛中大蒜素含量分别为(1 974.46±95.52)μg、(1 047.32±53.79)μg,仅显著高于对照组,相对释放率分别为67.8%、82.9%,其他时间点的羊毛中大蒜素含量与对照组无显著差异。对不同处理组大蒜素释放曲线进行拟合,结果显示一级方程拟合度最佳,在0~18 d内进行积分,A组积分面积为1 450.64,小于其他处理组。结果表明,A、B、C组3个大蒜素长效驱避剂配方制剂均能延缓大蒜素的释放,A组和B组可在12 d内延缓大蒜素的释放,而C组的缓释期只有2 d;A组的缓释效果最好,其次为B组。

The slow release properties of three allicinIxodes repellents(A,B and C),and their difference from ordinary allicin emulsion were studied. The first step was to establish a gas chromatography method for the determination of allicin in wool. The extraction time,extraction volume,extraction temperature and soaking time of wool in repellent which influence of allicin detection were optimized and screened. The method was used to detect the content of allicin in wool soaked with corresponding repellent at 0 d,1 d,2 d,3 d,5 d,8 d,12 d and 18 d. Taking the allicin content measured in wool on the0 d as the initial value and other time points as the residual value,the time/relative release rate curve was drawn,and the difference of allicin content in different treatment groups at the same time point was analyzed to evaluate the sustained-release performance of the three kinds of allicin repellent. The test wool was soaked in allicin water emulsion for 15 min,and 3 mL in absolute ethanol at 15 min at 35℃,the peak area of allicin in the extract was the largest,which was conducive to its quantitative detection. The content of allicin per gram of wool in group A was(4 181.93±201.89) μg,(2 317.84±113.12) μg,(1 662.96±96.03)μg and(1 037.51±32.07)μg at 1,2,3 and 5 d,respectively,which was significantly higher than that of other treatment groups,and the relative release rate of allicin was 31.3%,61.9%,72.7% and 82.9%,respectively;the content of allicin per gram of wool in group B was(3 324.70±194.78)μg,(1 691.17±131.46)μg and(764.03±6.75)μg at 1,2 and 5 d,respectively,which was significantly higher than those in group C and control(P<0.05),and the relative release rate was 46.6%,72.9% and 87.7%,respectively;the contents of allicin per gram of wool in group C were(1 974.46±95.52)μg and(1 047.32±53.79) μg on day 1 and day 2 respectively,which were significantly higher than those in the control group,and the relative release rates were 67.8% and 82.9%,respectively. There was no significant difference in allicin content with the control groups at other time points. The allicin release curves of different treatment groups were fitted. The results showed that the first-order equation was the best,and the integration area of group A was 1 450.64,which was smaller than that of other treatment groups. The long-term repellent formulations of allicin in three treatment groups A,B and C could delay the release of allicin,group A and group B could delay the release of allicin within 12 days,while group C had only 2 days;group A had the best sustained-release effect,followed by group B.