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4
Qualitative and Quantitative Analysis of Contaminants of Emerging Concernin Biosolids Using Dilute-and-Shoot UHPLC-Orbitrap MS Method
Conclus
Quantitati
Semi-qua
products i
Efforts to
Acknow
Dr. Ahmed Most
his postdoctal fel
te
™
3000 HPLC
nd a TCC-3400
s into a Thermo
00 mm column,
s. Three HPLC
FIGURE 1. Optimization of extraction solvent
min
/CH
3
OH:H
2
O
, pH 6.95
±
0.3
Curve
5
5
7
5
5
TABLE 2. Method performance for targeted compound analysis. MDL (method
detection limit) is derived from eight replicate spikes. (RSD: relative standard
deviation; REC: recovery)
Microsoft
®
and Excel
®
Scientific and its subs
Chemspider is a trade
This information is not
property rights of othe
Current extraction procedure has been validated for the analysis of 49 targeted
compounds. Table 2 showed the performance data for these 49 PPCPs.
Quantitative Determination of PPCPs in Biosolids Samples
Quantitative determination of targeted PPCPs in biosolids are shown in Table 3. Five
compounds, i.e., bisphenol A, caffeine, CBZ, TCC and TCS, were found in all six samples
at the high ppb range.
Table 4 showed targeted screening results from the same samples with 100%
trap
™
MS using
m was tuned and
s of MSCAL5
5 L/min). Spray
respectively.
ull-width-at-half-
ec when using
sec.
ntitative analysis
rgeted screening
heir metabolites,
hosphorus flame
ention time (RT)
n window (MEW)
database using
d (M-H)
−
quasi-
und. Those non-
ly 25
–
50 pg/mL
otopic mass (M)
±
10% from the
rom TraceFinder
e to carry out a
:H
2
O (0.1%
H
2
O (0.1%
owed similar
tion step used
Compound
Bisphenol A
Caffeine
Carbamazepine
Clofibric acid
DEET
Esterone
Estriol
Lidocaine
Oxybenzone
Triclocarban*
Triclosan*
TABLE 3. Result
*Semi-quantitat
TABLE 4. Result
Compound Name
Ethofumesate
Fenofibric-Acid
Metoprolol
Neotame
Spiroxamine
Sucralose
4-Chloro-2-(2,4-dic
4- & 6-Chloro-triclo
Acridine
acridone-N-carbald
Benzotriazol
Benzyldimethyldod
Benzyldimethylhex
Benzyl-dimethyl-tetr
Carbamazepin-10,1
Carbamazepine-10,
Dibutyl Phthalate
Didecyldimethylam
Diethyl Phthalate
Diethylhexyl Phthal
Compound
RSD
MDL
Rec
Compound
RSD
MDL
Rec
19-Norethisterone
10
27
75 Hydrocortisone
41
42
56
Acetamidophenol
2.4
21
57 Ibuprofen
3.7
51
114
a
-Estradiol
13
572
112 Indomethacin
4.6
15
92
a
-Ethynyl Estradiol
3.9
68
97 Ketoprofen
16
18
64
Atenolol
4.7
39
91 Lidocaine
8.4
6
73
b
-Estradiol
3
121
98 Lincomycin HCl
7.4
11
80
Bisphenol A
20
135
76 Naproxen
13
44
95
Caffeine
9.9
26
72 Norfloxacin
9.9
27
76
Carbadox
16
99
88 Ofloxacin
6.1
39
89
Carbamazepine
8.2
6
80 Oxolinic Acid
8.7
63
100
Chloramphenicol
5.6
7
73 Oxybenzone
14
14
54
Chlorotetracycline
9.3
110
132 Oxytetracycline HCl
8.3
57
128
Ciprofloxacin
5.6
35
88 Progesterone
5.9
20
96
Clofibric acid
1.9
7
94 Roxithromycin
13
65
141
DEET
16
10
67 Sulfachloropyridazine
10
14
76
Diazepam
8
33
57 Sulfadiazine sodium
15
269
50
Diclofenac sodium
6.6
16
88 Sulfadimethoxine
9.4
11
66
Doxycycline HCl
15
94
87 Sulfamerazine
17
22
73
Enrofloxacin
10
56
78 Sulfamethazine
7.1
9
74
Equilin
3.9
20
98 Sulfamethizole
6.7
9
74
Esterone
2.8
23
93 sulfamethoxazole
7.1
12
91
Estriol
9.6
81
94 Sulfathiazole
9.4
13
80
Gemfibrozil
12
15
116 Trimethoprim
20
70
98
Glipizide
7.7
9
78 Tylosin
9.9
287
97