Synthesis of meso-tetra-(3,5-dibromo-4-hydroxylphenyl)- porphyrin and its application to second-derivative spectrophotometric determination of lead in clinical samples
Zj. Li et al., Synthesis of meso-tetra-(3,5-dibromo-4-hydroxylphenyl)- porphyrin and its application to second-derivative spectrophotometric determination of lead in clinical samples, ANALYST, 124(8), 1999, pp. 1227-1231
A new very sensitive and selective chromogenic reagent, meso-tetra-(3,5-dib
romo-4-hydroxylphenyl)porphyrin [T(DBHP)P], was synthesized and studied for
the determination of trace lead in detail. In 0.10 mol l(-1) NaOH medium,
lead reacts with T(DBHP)P to form a 1∶2 yellow complex, which gives a
maximum absorption at 479 nm; 0-0.48 mu g ml(-1) Pb(II) obeyed Beer's law.
The molar absorptivity of the complex and Sandell's sensitivity are 2.5 x
10(5) l mol(-1) cm(-1) and 0.000812 mu g cm(-2), respectively. Second-deriv
ative spectrophotometry is better than conventional spectrophotometry in se
nsitivity and selectivity, and its limit of quantification, limit of detect
ion and relative standard deviation are 0.70 ng ml(-1), 0.21 ng ml(-1) and
1.0%, respectively. Ca (3250-fold), Mg (2000-fold), Sr (1000-fold), Ba (750
-fold), Al (1000-fold), Bi (500-fold), Fe (2000-fold), Co (750-fold), Ni (1
000-fold), Cu (750-fold), Zn (1250-fold ), Cd (2500-fold) and Ag (550-fold)
do not interfere with the determination of lead. The chromogenic system is
remarkably superior to other reagents, especially porphyrin compounds. The
influence caused by oxygen in air or in solution can be easily eliminated
by adding Na2SO3. The reaction is very stable, the stability constant of th
e complex being 1.2 x 10(45). The chromogenic reaction is completed within
1 min at room temperature when 8-hydroxylquinoline is used as catalyst. The
proposed method has been applied to the direct determination of trace lead
in clinical samples. The accuracy and precision are both very satisfactory
.