添加量(ng/mg) |
绝对回收率 |
CV(%) |
相对回收率 |
CV(%) |
|
AMP |
5 |
96.39 |
4.11 |
106.48 |
8.93 |
20 |
78.44 |
16.23 |
88.32 |
15.77 |
|
MAMP |
5 |
95.33 |
6.34 |
104.92 |
5.74 |
20 |
79.16 |
16.27 |
89.04 |
14.33 |
|
4-PBA |
1μg |
88.80 |
7.76 |
2.5 线性关系与最低检出限
准确取不同量的AMP、MAMP标准品,分别加至10mg空白毛发中,加入内标,配成系列标准样品,然后按样品处理项操作,分别用GC/NPD和GC/MS分析,毛发中AMP、MAMP的浓度与AMP、MAMP与内标的峰面积比成线性关系,其线性范围及最低检出限见表2。
表2 毛发中AMP、MAMP的线性关系及最低检测限
仪器方法 |
样品 |
回归方程 |
线性范围(ng/mg) |
最低检出限(ng/mg) |
GC/NPD |
AMP |
y=0.0051x+0.0228r=0.9967 |
1~50 |
0.5 |
MAMP |
y=0.0113x+0.0297r=0.9969 |
1~50 |
0.5 |
|
GC/MS |
AMP |
y=0.0041x+0.0003r=0.9978 |
0.1~15 |
0.1 |
MAMP |
y=0.0075x+0.0017r=0.9990 |
0.1~15 |
0.1 |
2.6 染毒豚鼠毛发中MAMP及其代谢产物AMP浓度变化过程的测定
2.6.1 单次注射MAMP豚鼠毛发中MAMP及AMP浓度变化过程
给豚鼠腹腔单次注射MAMP(30mg/kg,n=6,背部黑色毛发,给药前剃光),每天剃毛,连续10天,所得毛发按样品处理项操作,测定MAMP及其代谢产物AMP的含量,结果如图5所示。在给药后第二天MAMP及其代谢产物AMP的含量达到峰值,第五天后测不出MAMP,第七天以后测不出AMP。整个时间过程中,代谢产物AMP的含量均大于原体MAMP。
2.6.2 多次注射MAMP豚鼠毛发中MAMP及AMP浓度变化过程
给豚鼠腹腔注射MAMP(20mg/kg,隔天一次,连续7次,n=6,背部黑色毛发,给药前剃光),隔天剃毛,连续10次,所得毛发按样品处理项操作,测定MAMP及其代谢产物AMP的含量,结果如图6所示。图中可见,首次给药后第十四天MAMP及其代谢产物AMP的含量达到峰值,第二十天以后测不出MAMP和AMP。整个时间过程中,代谢产物AMP的含量也均大于原体MAMP。
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