110 / 302
MS
MS analysis was carried out on a Thermo Scientific TSQ
Vantage triple stage quadrupole mass spectrometer. Two
selected reaction monitoring (SRM) transitions per com-
pound were acquired: one for quantitation and the other
for positive confirmation. To maximize the performance
of the triple stage quadrupole, time-specific SRM “win-
dows” were employed at the retention times of the target
compounds.
Results and Discussion
The current EPA Method 1694 describes three different
LC methods for PPCPs from Groups 1, 2, and 4, which are
amenable to positive electrospray ionization (ESI) MS/MS.
To simplify the method and reduce the total analysis time,
a single 10-minute LC-MS/MS method was developed,
which included compounds from additional pharmaceuti-
cal classes not included in EPA Method 1694, such as
beta-blockers. In total, 67 compounds were analyzed by
positive ESI-MS/MS (Table 1). Of these, 54 were from EPA
Method 1694 Groups 1, 2, and 4.
Table 1. PPCPs analyzed
Compound
Class
Compound
Class
Trimethoprim
Antibiotic
4-epi-Chlorotetracycline
Antibiotic, tetracycline
Cefotaxime
Antibiotic, cephalosporin
Demeclocycline
Antibiotic, tetracycline
Norfloxacin
Antibiotic, fluoroquinolone
Chlorotetracycline
Antibiotic, tetracycline
Ofloxacin
Antibiotic, fluoroquinolone
Doxycycline
Antibiotic, tetracycline
Ciprofloxacin
Antibiotic, fluoroquinolone
Anhydrotetracycline
Antibiotic, tetracycline
Lomefloxacin
Antibiotic, fluoroquinolone
Carbamazepine
Anticonvulsant
Enrofloxacin
Antibiotic, fluoroquinolone
Fluoxetine
Antidepressant
Sarafloxacin
Antibiotic, fluoroquinolone
Miconazole
Antifungal
Flumequine
Antibiotic, fluoroquinolone
Thiabendazole
Antihelmintic
Lincomycin
Antibiotic, macrolide
Diphenhydramine
Antihistamine
Azithromycin
Antibiotic, macrolide
Acetaminophen
Analgesic
Erythromycin
Antibiotic, macrolide
Codeine
Analgesic, narcotic
Tylosin
Antibiotic, macrolide
Cimetidine
Antiacid reflux
Anhydroerythromycin Antibiotic, macrolide
Ranitidine
Antiacid reflux
Clarithromycin
Antibiotic, macrolide
Digoxigenin
Antiarrythmic
Roxithromycin
Antibiotic, macrolide
Digoxin
Antiarrythmic
Ampicillin
Antibiotic, penicillin
Diltiazem
Antiarrythmic, benzothiazepine
Penicillin G
Antibiotic, penicillin
Dextromethorphan**
Antitussive
Penicillin V
Antibiotic, penicillin
Atenolol
Beta-blocker
Oxacillin
Antibiotic, penicillin
Metoprolol
Beta-blocker
Cloxacillin
Antibiotic, penicillin
Propranolol
Beta-blocker
Metformin*
Antidiabetic
Albuterol
Bronchodialator
Sulfadiazine
Antibiotic, sulfa
Midazolam
Sedative, benzodiazepine
Sulfathiazole
Antibiotic, sulfa
1-OH Midazolam
Sedative, benzodiazepine
Sulfamerazine
Antibiotic, sulfa
1-OH Alprazolam
Sedative, benzodiazepine
Sulfamethazine
Antibiotic, sulfa
Alprazolam
Sedative, benzodiazepine
Sulfamethizole
Antibiotic, sulfa
Nordiazepam
Sedative, benzodiazepine
Sulfachloropyridazine Antibiotic, sulfa
1,7-Dimethylxanthine
Stimulant
Sulfamethoxazole
Antibiotic, sulfa
Caffeine
Stimulant
Sulfadimethoxine
Antibiotic, sulfa
Benzoylecgonine
Stimulant
Minocycline
Antibiotic, tetracycline
Cocaine
Stimulant
Oxytetracycline
Antibiotic, tetracycline
Cocaethylene
Stimulant
4-epi-Tetracycline
Antibiotic, tetracycline
Cotinine
Stimulant
Tetracycline
Antibiotic, tetracycline
*Metformin was analyzed using HILIC
**PPCPs not included in EPA 1694